PLANT DESIGN

6.1
6.1.1 6.1.2

Laboratory Preparation of Bio Diesel

Equipment needed: Four 500 ml Erlenmeyer flasks containing 200 g of egetable oil Four 125 ml Erlenmeyer flasks! " containing #" g of met$anol! one containing 21.5 g of met$anol Four $ot plate%stirrers Four separatory funnels &it$ ringstan's (luminum foil )for capping flasks* +mall bottles containing pre&eig$e' so'ium $y'ro,i'e! t$ree &it$ 2 g! one &it$ 10 g. Task

Group 1: -oo muc$ &ater +tarting &it$ 200 g of egetable oil in a 500 ml flask. ('' 10 g of &ater. ('' 2 g of so'ium $y'ro,i'e pellets to #" g of met$anol an' agitate until t$e pellets are 'issol.e'. ('' t$e met$anol%so'ium $y'ro,i'e solution to t$e egetable oil. ('' a magnetic stirring bar an' place on t$e $ot plate. /eat to 6006512 an' agitate for 1 $our. Pour into a separatory funnel an' allo& separating. Group 2: -oo muc$ catalyst +tart &it$ 200 g of egetable oil in a 500 ml flask. ('' 10 g of so'ium $y'ro,i'e pellets to #" g of met$anol an' agitate until t$e pellets are 'issol.e'. /eating may be re3uire'. ('' t$e met$anol%so'ium $y'ro,i'e solution to t$e egetable oil. ('' a magnetic stirring bar an' place on t$e $ot plate. /eat to 6006512 an' agitate for 1 $our. Pour into a separatory funnel an' allo& separating. Group 3: 4ot enoug$ alco$ol +tart &it$ 200 g of egetable oil in a 500 ml flask. ('' 2 g of so'ium $y'ro,i'e pellets to 21.5 g of met$anol an' agitate until t$e pellets are 'issol.e'. /eating may be re3uire'. ('' t$e met$anol%so'ium $y'ro,i'e solution to t$e egetable oil. ('' a magnetic stirring bar an' place on t$e $ot plate. /eat to 6006512 an' agitate for 1 $our. Pour into a separatory funnel an' allo& separating.

52

Group 4: /ig$ free fatty aci' fee'stock +tart &it$ 200 g of animal fat in a 500 ml flask. ('' 2 g of so'ium $y'ro,i'e pellets to #" g of met$anol an' agitate until t$e pellets are 'issol.e'. ('' t$e met$anol%so'ium $y'ro,i'e solution to t$e animal fat. ('' a magnetic stirring bar an' place on t$e $ot plate. /eat to 6006512 an' agitate for 1 $our. Pour into a separating funnel an' allo& separating. Group 5: 6il E,traction from (lgae. Let t$e (lgae 'ry in o.en for 2 $ours. 7i, n0$e,ane an' rigi'ly stir. (long &it$ n0$e,ane mi,es take t$e algae oil. Let n0$e,ane e.aporate t$e rest &ill be algae oil.

5"

Fig 11: Laboratory wor at IESE !N"ST#

6.2

Propose' Bio Diesel Plant

Fig 12: Propo$%& 'io Di%$%( P(a)t

6.2.3

'a$i* P(a)t E+uip,%)t a)& -p%ratio)

-$e intent of t$e basic plant e3uipment an' operation section is to 'iscuss t$e principles be$in' t$e primary plant e3uipment t$at &oul' be use' in a bio'iesel pro'uction facility. 8nclu'e' &ill be 'iscussion of reactors )bot$ batc$ an' continuous types*! pumps! centrifuges! an' 'istillation columns. (lt$oug$ t$ere &ill be a''itional e3uipment in t$e plant suc$ as settlers! storage tanks! etc.! t$e four classes of e3uipment 'iscusse' $ere represent t$e $eart of t$e process. 6.2.3.1 Reactors -$e reactor is t$e only place in t$e process &$ere c$emical con.ersion occurs. -$erefore! it 'ictates &$at c$emical species must be $an'le' 'o&nstream of t$e reactor. 9eactors can be place' into t&o broa' categories! batc$ reactors an' continuous reactors. -&o of reactors &it$in t$e continuous reactor category are continuous stirre' tank reactors )2+-9s* an' plug flo& reactors )PF9s*. 8n t$e batc$ reactor! t$e reactants are c$arge' into t$e reactor at t$e 'etermine' amount. -$e reactor is t$en close' an' taken to t$e 'esire' reaction con'itions )temperature! pressure! an' stir rates*. -$e c$emical composition &it$in t$e reactor c$anges &it$ time. 6nce t$e prescribe' reaction time is complete! t$e c$emical contents of t$e reactor are remo.e' an' sent for subse3uent processing. 8n contrast! continuous reactors 5#

$a.e a stea'y flo& of reactants into t$e reactor an' pro'ucts out of t$e reactor. 6nce a continuous flo& reactor reac$es stea'ystate operation! t$e pro'uct composition lea.ing t$e reactor becomes constant. For 2+-9s! t$e reactants are fe' into a &ell0mi,e' reactor. -$e composition of t$e pro'uct stream is i'entical to t$e composition &it$in t$e reactor. /ol'0up time in a 2+-9 is gi.en by a resi'ence time 'istribution. For PF9s! t$e reactants are fe' into one si'e of t$e reactor. -$e c$emical composition c$anges as t$e material mo.es in plug flo& t$roug$ t$e reactor. -$e resi'ence time is 'efine' by t$e lengt$ of time re3uire' for molecules to tra.el t$roug$ t$e reactor. -$e most important consi'erations &it$in a reactor are t$e e,tent of reaction of t$e reactants! &$ic$ is kno&n as con.ersion! an' t$e selecti.ity of t$e reaction to t$e 'esire0' pro'ucts! &$ic$ is kno&n as t$e selecti.ity. :ey reactor .ariables t$at 'ictate con.ersion an' selecti.ity aretemperature! pressure! reaction time )resi'ence time*! an' 'egree of mi,ing. 8n general! increasing t$e reaction temperature increases t$e reaction rate an'! $ence! t$e con.ersion for a gi.en reaction time. /o&e.er! if more t$an one reaction is taking place! t$e selecti.ity to t$e 'esire' pro'ucts can be impacte' by c$anging t$e reaction temperature. 8n t$e transesterification reaction! t$e selecti.ity of t$e reaction is not negati.ely impacte' by increasing temperature. 8ncreasing temperature in t$e transesterification reaction 'oes impact t$e operating pressure. -$e reaction is a li3ui' p$ase reaction! so t$e pressure in t$e reactor must be maintaine' at a le.el t$at keeps t$e met$anol in t$e li3ui' p$ase. -$erefore! as t$e reaction temperature is increase' t$e pressure must also be increase'. (not$er means to increase t$e con.ersion in a reactor is to increase t$e reaction time. For a gi.en temperature! con.ersion &ill increase as t$e reaction time increases. 8ncreasing t$e reaction time $as t$e negati.e effect of 'ecreasing t$e c$emical t$roug$put in a gi.en plant or increasing t$e reactor si;e for a gi.en c$emical t$roug$put. ( final .ery important parameter in t$e reactor is t$e 'egree of mi,ing or mass transfer. For batc$ reactors an' 2+-9s t$e 'egree of mi,ing is 'irectly relate' to t$e amount of energy intro'uce' t$roug$ t$e impeller. 8ncreasing t$e spee' of t$e impeller! &$ic$ increases t$e energy input to t$e reactor! increases t$e 'egree of mi,ing! &$ic$ impro.es t$e performance of t$e reactor. ( t$res$ol' e,ists &$ere a''itional mi,ing &ill not pro.i'e any performance en$ancement. For PF9s! t$e 'egree of mi,ing is 'ictate' by t$e 'esign of t$e reactor an'%or catalyst use' &it$in t$e reactor! since no mi,ing 'e.ice is present in t$e reactor t$at can be in'epen'ently manipulate'. Batc$ reactors $a.e se.eral positi.e features inclu'ing goo' mi,ing c$aracteristics an' relati.e ease of $an'ling $omogeneous catalysts as use' in t$e bio'iesel transesterification reaction. (s mentione' abo.e! t$e reactant concentrations c$ange &it$ time in t$e reactor as 'oes t$e pro'uct concentration. -$erefore! t$e effect of reaction in$ibition by reaction pro'ucts suc$ as e,perience' &it$ glycerol can be minimi;e'. /o&e.er! batc$ reactors are generally not use' in t$e pro'uction of large .olume c$emicals since it is most efficient to operate t$e subse3uent separation an' purification steps in a continuous

55

mo'e. -$is batc$ to continuous mo'e can be o.ercome by using multiple reaction .essels se3uence' to gi.e effecti.ely continuous operation or by employing a large <surge= .essel after t$e reactor. 2+-9s! &$ic$ ob.iate t$e primary problem &it$ batc$ reactors! also pro.i'e goo' mi,ing c$aracteristics. /o&e.er! t$e uniform concentration present in t$e reactor gi.es a lo&er reaction 'ri.ing force an' can also ma,imi;e reaction in$ibition effects. PF9s or tubular reactors are t$e most common reactors in t$e c$emical in'ustry. Despite being continuous! t$e reactant concentration in t$ese reactors c$anges &it$ 'istance 'o&n t$e be' to ma,imi;e t$e 'ri.ing force for t$e reaction! &$ic$ is similar to a batc$ reactor. (c$ie.ing goo' mi,ing can be more problematic &it$ PF9s an' t$ese type of reactors typically use soli' catalysts. 6.2.3.2 Pumps >$ile t$e role of pumps in a c$emical plant seems rat$er mun'ane! t$ey play t$e key role in mo.ing c$emicals t$roug$ t$e manufacturing plant. -$e most common type of pump in t$e c$emical in'ustry is a centrifugal pump. 8n many applications! t$e flui' s$ear intro'uce' by a centrifugal pump is not a point of concern. /o&e.er! t$e s$ear create' by a centrifugal pump can create emulsion problems for t$e pro'uct stream from t$e bio'iesel reactor. -$e amount of flui' s$ear imparte' by t$e pump can be significantly re'uce' by using a positi.e 'isplacement pump. -$ere are a number of 'ifferent types of positi.e 'isplacement pumps inclu'ing gear pumps )e,ternal an' internal* an' lobe pumps. E,ternal gear pumps generally $a.e t&o gears &it$ e3ual number of teet$ locate' on t$e outsi'e of t$e gears! &$ereas! internal gear pumps $a.e one larger gear &it$ internal teet$ an' a smaller gear &it$ e,ternal teet$. -$e li3ui' is <pumpe'= from t$e action of being carrie' bet&een t$e gear teet$ follo&e' by 'isplacement as t$e teet$ mes$. 8n most e,ternal gear pumps! one gear 'ri.es t$e ot$er. -$e internal gear pump $as t$e a'.antage of fe&er mo.ing parts! but it cannot $an'le li3ui' streams containing soli's or abrasi.es. Lobe pumps impart less s$ear to t$e flui' being pumpe' t$an gear pumps. -$e lobes in t$e pump are 'esigne' for no contact! so timing gears are re3uire' for eac$ lobe. -$erefore! t$e lobe pump $as more mo.ing parts t$an gear pumps. Lobe pumps are best for $an'ling <fragile= an' $ig$ .iscosity flui's at lo& pressures. (s &it$ gear pumps! lobe pumps &ork by carrying t$e flui' bet&een lobes follo&e' by 'isplacement as t$e lobes come toget$er. +ince t$e lobes are 'esigne' for no contact! fairly $ig$ amounts of slip can occur if t$e flui' to be pumpe' $as lo& .iscosity. 2entrifugal pumps con.ert .elocity into feet of $ea' &$ere t$e feet of $ea' is in'epen'ent of t$e 'ensity of t$e li3ui' being pumpe'. /o&e.er! con.ersion of t$e feet of $ea' to output pressure re3uires inclusion of t$e flui' 'ensity. For e,ample! 2"1 feet of &ater in a column! i.e.! 2"1 feet of $ea'! e,erts a pressure of 100 psig at t$e base! &$ereas t$e same 2"1 feet of bio'iesel &it$ specific gra.ity of 0.?? &oul' e,ert a pressure of ?? psig. -$erefore! t$e 'isc$arge pressure of t$e pump &$en pumping &ater &oul' be $ig$er t$an &it$ bio'iesel. -$e primary components of a centrifugal pump are )1* a s$aft! )2* a coupling attac$ing t$e s$aft to a motor! )"* bearings to support t$e s$aft! )#* a seal aroun' t$e s$aft to pre.ent leakage! )5* an impeller! an' )6* a .olute! &$ic$

56

con.erts t$e kinetic energy imparte' by t$e impeller into feet of $ea'. -$e role of t$e impeller is to increase t$e kinetic energy of t$e li3ui'. -$e li3ui' enters an' lea.es t$e impeller at t$e same pressure. (s t$e li3ui' flo&s t$roug$ t$e .olute! t$e .elocity is 'ecrease' &it$ t$e energy transferre' to pressure.

Fig 13: .%)tri/uga( Pu,p

>$ile leaking pump seals or impeller &ear can be operational issues &it$ pumps! t$e most common issue &it$ pumps is t$e loss of suction pressure. +uction pressure is t$e pressure supplie' to t$e suction si'e of t$e pump by t$e li3ui'. During loss of suction pressure! &$ic$ is kno&n as ca.itation! t$e pump 'isc$arge pressure an' t$e 'isc$arge flo& rates become erratic an' lo&. 2a.itation is create' by .apori;ation of li3ui' at t$e pump suction. -$is situation can be create' be a plug in t$e suction piping or by starting t$e pump up too rapi'ly. 8n general! positi.e 'isplacement pumps are more 'ifficult to ca.itate t$an centrifugal pumps. 2entrifuges are most typically use' to separate soli's an' li3ui's! but t$ey can also be use' to separate immiscible li3ui's of 'ifferent 'ensities. -$is type of separation can also be ac$ie.e' using a settling tank. >$ile a settling tank may be c$eaper! a centrifuge can be use' to increase t$e rate of separation relati.e to a settling tank. 8n a centrifuge t$e separation is accomplis$e' by e,posing t$e mi,ture to a centrifugal force. -$e more 'ense p$ase &ill be preferentially separate' to t$e outer surface of t$e centrifuge. ( centrifuge generally consists of !1# ( bo&l containing t$e mi,ture! !2# ( 'ri.e s$aft an' 'ri.e0s$aft bearings! !3# ( 'ri.e mec$anism! an' !4# ( casing to segregate t$e separate' pro'ucts.

55

Fig 14: .%)tri/ug%$

-$e performance of a centrifuge 'epen's on t$e specifications of t$e centrifuge as &ell as t$e c$aracteristics of t$e mi,ture to be separate'. >$ile centrifuges are generally rate' in terms of mi,ture $an'ling capacity! t$e pro'uct 3uality specifications are t$e most important consi'eration. -$e c$oice of appropriate centrifuge type an' si;e are pre'icate' on t$e 'egree of separation nee'e' in a specific system. -$e .iscosity of t$e li3ui' $as important implications on t$e c$oice of centrifuge si;e since $ig$er .iscosity flui's are more 'ifficult to $an'le. 8f a sufficient 'ensity 'ifference e,ists bet&een immiscible flui's! centrifugation is a faster means of separation t$an settling. 6.2.3.3 Distillation (not$er means of separating c$emicals in a flui' mi,ture is by e,ploiting t$e 'ifferences in boiling points bet&een t$e c$emicals. 8f t$e boiling points are sufficiently 'ifferent for t$e c$emicals to be separate'! suc$ as &it$ &ater an' bio'iesel! an e.aporator or flas$ .apori;er can be use' for t$e separation. 8n t$e e.aporator! t$e li3ui' is $eate' to a temperature in &$ic$ only t$e more .olatile c$emical species &ill .apori;e. (s suc$ t$e .apor stream lea.ing t$e .aporator &ill be enric$e' in t$e more .olatile species an' t$e li3ui' stream from t$e e.aporator &ill be enric$e' in t$e less .olatile species. 8n an e.aporator! t$e separation is accomplis$e' by supplying $eat &$ile t$e mi,ture is $el' at a fi,e' pressure. 8n contrast! a flas$ .apori;er first $eats t$e li3ui'! at an ele.ate' pressure. -$en! t$e $eate' li3ui' is sent t$roug$ a flas$ .al.e t$at 'ecreases t$e pressure. -$e 'ecrease in pressure causes t$e more .olatile portion of t$e li3ui' mi,ture to .apori;e. (n important separation 'e.ice for miscible flui's &it$ similar boiling points )e.g.! met$anol an' &ater* is t$e 'istillation column. +eparation in a 'istillation column is pre'icate' on t$e 'ifference in .olatilities )boiling points* bet&een c$emicals in a li3ui' mi,ture. 8n a 'istillation column t$e concentrations of t$e more .olatile species are enric$e' abo.e t$e fee' point an' t$e less .olatile species are enric$e' belo& t$e fee' point. -$e .apori;ation in t$e column is 'ri.en by $eat supplie' in t$e reboiler! &$ic$ is subse3uently remo.e' in t$e o.er$ea' con'enser. -$e temperature in t$e 'istillation column is t$e $ig$est at t$e bottom an' 'ecreases mo.ing up t$e column. Distillation columns can use eit$er trays or packing. -$e 'egree of separation t$at can be ac$ie.e' in a 'istillation column is 'ictate' by t$e relati.e .olatilities of t$e c$emicals to be separate'! t$e number of trays or t$e $eig$t of t$e packing! an' t$e reflu, ratio. 2$emicals &it$ .ery 'ifferent boiling points are easier to separate t$an t$ose &it$ similar boiling points. 8ncreasing t$e number of trays or t$e $eig$t of packing can increase t$e amount of separation. 9eflu, ratio is t$e amount of con'ense' o.er$ea' .apor t$at is fe' back into t$e top of t$e column. 8ncreasing t$e reflu, ratio increases t$e 'egree of separation. 8ncreasing t$e number of trays or $eig$t of packing increases t$e column $eig$t an' increasing t$e reflu, ratio increases t$e column 'iameter. Eit$er of t$ese increases in column 'imensions increases t$e capital cost of t$e column.

5?

-raye' 'istillation columns are t$e most common. ( tray is &$ere contacting occurs bet&een t$e .apor stream an' t$e li3ui' stream. -$e li3ui' enters t$e fee' tray t$roug$ t$e 'o&ncomer from t$e abo.e tray! flo&s across t$e tray &$ere is interacts &it$ t$e .apor! spills o.er a &eir! an'! finally! flo&s t$roug$ t$e 'o&ncomer to t$e ne,t tray. -$e .apor flo&s up t$roug$ $oles in t$e tray. 8t is important to $a.e appropriate flo& rates of t$e li3ui' an' .apor to get optimal column operation. 8f t$e li3ui' flo& rates become too $ig$! poor contacting occurs &it$ t$e .apor an' in t$e e,treme floo'ing of t$e column can occur. -$e onset of floo'ing in a column is easy to obser.e since t$e column pressure 'rop &ill increase marke'ly &$en floo'ing begins. 8f t$e .apor flo& rate is too $ig$! li3ui' can be entraine' an' carrie' o.er to t$e abo.e tray lea'ing to poorer separation. 8n contrast! too lo& of a .apor rate can lea' to &eeping of t$e li3ui' t$roug$ t$e tray! &$ic$ 'iminis$es t$e separation. -$e li3ui' an' .apor flo& rates are 'ictate' by t$e operation of t$e reboiler an' t$e con'enser! &$ic$ means t$ey are controlle' by t$e energy input an' remo.al. -$e materials of construction is an important consi'eration for t$e reactor an' storage tanks. -$e 'eman's on t$e materials use' for t$e storage tanks 'o&nstream of t$e reactor are lo&er since t$ese tanks contain nearly p/ neutral c$emicals. -$e materials of construction for t$e storage tanks are 'iscusse' in t$e -ransportation an' +torage section. 8n contrast! t$e materials of construction re3uire' in t$e reactor must &it$stan' basic con'itions for t$e transesterification reaction or aci'ic con'itions if an esterification approac$ is use' to con.ert free fatty aci's. For t$e base0cataly;e' transesterification reaction! stainless steel is t$e preferre' material for t$e reactor. /o&e.er! stainless steel &ill not be goo' c$oice for use in t$e aci'0cataly;e' esterification reaction because stainless steel is sub@ect to attack by aci's. An'er t$ese con'itions! an aci' resistant material suc$ as /astelloy s$oul' be use' for t$e reaction .essel. 6.2.4 .0%,i*a( P(a)t .o)tro($

-o pro'uce 3uality pro'ucts from a bio'iesel pro'uction plant it is necessary to be able to control t$e pro'uction process. >$ile a tremen'ously important control .ariable is t$e properties of t$e fee'stock to t$e process! t$is section &ill only 'iscuss t$e control of c$emical plants &it$in t$e unit operation of t$e processes! suc$ as t$ose 'iscusse' in t$e pre.ious section. -&o general types of processes can be use' in t$e pro'uction of bio'iesel! eit$er batc$ or continuous. For batc$ processes t$e process control .ariables &ill be temperature! pressure! an' le.els. -emperature an' pressure control are critical &it$in t$e reaction an' separation sections of t$e plants. Le.el control 'ictates c$arging to t$e reactor! operation of separation 'e.ices! an' pro'uct storage. For continuous processes t$e process control .ariables inclu'e temperature! pressure! le.el! an' flo& rate. 8t is important to note t$at process .ariables! &$ic$ are monitore' an' controlle'! are not t$e same as t$e pro'uct specifications. +pecifications are properties t$at are re3uire' of t$e final pro'uct suc$ as t$ose gi.en in (+-7 D 6551 for bio'iesel. 2ontrol .ariables are t$ose process .ariables t$at are monitore' an' a'@uste' to meet t$e 'esire' specifications. (s suc$! specifications are generally measure' off0line in an analytical laboratory! &$ile t$e process .ariables are process con'itions t$at are measure' in real time.

5B

-$e process .ariables are relate' to t$e specifications t$roug$ some type of process mo'el. -$e process mo'el &ill typically be pro.i'e' by t$e process licensor &it$ subse3uent refinement from plant operation e,perience. +ome manufacturing plants &ill 'e.elop t$eir o&n statistical or empirical mo'els. 8t s$oul' be note' t$at t$e process mo'els are typically fee'stock 'epen'ent. 8n 'iscussing process .ariable measurement instruments! t$e performance of t$e instruments can be c$aracteri;e' by t$eir accuracy an'%or precision. (ccuracy is t$e ability of an instrument to measure t$e correct or <true= .alue of a process .ariable. 8n contrast! precision is t$e ability of an instrument to repro'uce a process .ariable .alue &it$in a certain inter.al. (s suc$! it is possible to $a.e eit$er <accurate an' imprecise= or <inaccurate an' precise= instruments. For 'ay0to0'ay operation t$e ability of a measurement instrument to be precise is generally more important t$an t$e nee' to be accurate. /o&e.er! &$en t$e measurement instrument nee's to be replace'! accuracy becomes an important issue. >$en consi'ering an instrumental control system for a c$emical plant t$ere are a number of factors t$at s$oul' be consi'ere'C cost! precision! reliability! an' operator interface. 8t is 'esirable to $a.e t$e lo&est cost monitoring system t$at &ill allo& appropriate control of t$e process. Precision is important to assure t$at t$ere is repro'ucibility of measurements. 9eliability insures t$at t$e system is not prone to failures. Finally! it is 'esirable to $a.e a monitoring an' control system t$at pro.i'es an easy interface &it$ t$e plant operators. 6.2.4.1 Temperature Measurement -$e most common process .ariable monitore' in a c$emical plant is t$e temperature. -$e temperature at a specific point is generally measure' using t$ermocouples! &$ic$ are electrical 'e.ices. -$ermocouples are ma'e of t&o 'ifferent metallic &ires. -$ese &ires are connecte' at a @unction. (n electrical current is establis$e' &$en t$e @unction is $eate'. -$e electrical current is proportional to t$e temperature at t$e @unction. For t$is reason! t$e t$ermocouple must be calibrate' to correlate temperature to current.

Fig 15: T0%r,o*oup(%

?0

-$ermocouples are categori;e' by t$e metals use' in t$eir @unctions! &it$ 'ifferent metal @unction combinations being more appropriate for 'ifferent temperature ranges. 8n'i.i'ual t$ermocouples are typically not calibrate' by t$e supplier. 8nstea'! manufacturers &ill typically test a representati.e portion of t$e t$ermocouples t$ey pro'uce. Due to t$e manufacturing proce'ure! t$ermocouples are usually precise )or completely 'onDt &ork* but can be inaccurate. -$e t$ermocouple is typically enclose' &it$in a t$ermo &ell. -$e t$ermocouple must be fully inserte' into t$e t$ermo &ell &it$ t$e t$ermo &ell e,ten'e' appropriately into t$e process to obtain a correct rea'ing. 8f t$e temperature of a process li3ui' is being measure' it is generally a'e3uate for t$e t$ermo &ell to e,ten' about 20" inc$es into t$e li3ui'. Due to inferior $eat transfer! t$e t$ermo &ell s$oul' e,ten' about 6 inc$es into a process .apor. -$ermocouples are typically use' in processes for bot$ monitoring an' controlling t$e process. >$en a t$ermocouple is use' as part of a process control loop! t$e electrical current output from t$e t$ermocouple is compare' &it$ t$e current e,pecte' for t$e set point temperature. De.iation of t$e actual temperature from t$e set point temperature &ill cause a c$ange in t$e output to a $eater or cooler t$at is inclu'e' in t$e control loop. 6.2.4.2 Pressure Measurement: Pressure .alues can be measure' using se.eral 'ifferent types of 'e.ices suc$ as li3ui' column! elastic element! an' electrical sensing. -$e most common form of a li3ui' column 'e.ice is a manometer in &$ic$ t$e li3ui' $eig$t can be obser.e' .isually an' correlate' to t$e pressure t$roug$ t$e 'ensity of t$e li3ui'. Li3ui' column 'e.ices are rarely use' in c$emical processes. Elastic element 'e.ices measure pressure by 'etermining 'eformation of an elastic material. -$is elastic material is usually metallic. 6ne type of elastic element 'e.ice uses bello&s elements. -$e 'isplacement of t$e bello&s can be correlate' to t$e pressure .alue. -$e most common pressure measurement instruments use' in c$emical processes are electrical sensing 'e.ices! &$ic$ are kno&n as strain gauges. +train gauges are pre'icate' on t$e fact t$at t$e electrical resistance of con'ucting soli's c$anges &it$ lengt$ an' 'iameter of t$e soli'. -$e 'imensional c$anges of t$e soli' in'uce' by a pressure cause an increase in t$e electrical resistance of t$e con'ucting soli'. (n elastic element or electrical sensing 'e.ice use' to measure pressure is calle' a pressure trans'ucer.

Fig 16: Pr%$$ur% Tra)$&u*%r

?1

-$e pressure tap for a trans'ucer s$oul' be locate' in t$e .apor p$ase of a process. ( trans'ucer locate' in t$e li3ui' p$ase &ill 'etect a 'ifferent pressure at 'ifferent 'ept$s in t$e li3ui'. -o use a pressure trans'ucer for process control or in continuous monitoring! t$e trans'ucer must pro'uce an electrical signal. For t$e elastic element 'e.ice! t$e 'irect pressure rea'ing 'ue to 'isplacement must some$o& be con.erte' to an electrical signal. (n a'.antage of t$e electrical sensing approac$ is t$at t$ese 'e.ices 'irectly pro.i'e an electrical signal. (s &it$ t$ermocouples! pressure trans'ucers can be use' for process control by comparing t$e measure' pressure to a 'esire' set point pressure. 6.2.4.3 Level measurement: Le.el measurement can be use' to yiel' mass balance information across t$e process or loa'ing in a batc$ reactor. /istorically! le.el measurement 'e.ices $a.e typically been 'isplacer0base' meters or 'ifferential pressure meters. -$e 'isplacer0base' meter is base' on buoyancy. -$e 'isplacer is immerse' in a 'isplacer c$amber t$at is locate' as a si'e c$amber. -$e 'isplacer is restraine' by an elastic element &$ose motion is proportional to t$e buoyant force! so t$e le.el can be 'etermine' by t$e .ertical location of t$e 'isplacer. Differential pressure meters! &$ic$ are t$e most common le.el in'icating 'e.ices! measure t$e 'ifference in pressure bet&een t&o pressure taps in a .essel. 8t is important to note t$at bot$ of t$ese le.el measurement in'icators are li3ui' 'ensity 'epen'ent! so t$at c$anges in li3ui' 'ensities can affect t$eir rea'ings. -$is effect can be particularly important if se.eral li3ui' p$ases are present in t$e 'e.ice. For e,ample! t$e $eig$t of li3ui' in a gauge glass connecte' to a .essel is not a 'irect measurement of t$e li3ui' le.elE 9ecently! le.el measurement 'e.ices $a.e been 'e.elope' t$at use signal reflectance from an ultrasonic trans'ucer or ra'io fre3uency! &$ic$ measures t$e c$ange in impe'ance bet&een t&o capacitor electro'es.

Fig 11: L%2%( ,%a$ur%,%)t

8n a''ition to 'ensity! t$ere are a number of factors t$at can influence t$e reliability of a le.el measurement. Plugge' taps can occur &it$out causing apparent 'iscrepancies in t$e le.el measurement 'e.ice. E,cursions to $ig$ li3ui' le.els can impact t$e reliability of t$e le.el measurement as can t$e presence of foam in t$e .essel. -$e measurement an' control of le.el in a .essel generally re3uires t&o taps into t$e .essel. 8t is important t$at t$ese taps are properly .al.e'. +ince t$e le.el in'icator can be ?2

use' to monitor t$e amount of material in a .essel! it can be use' to track c$emical in.entory &it$in t$e process as &ell as to control t$e c$arging of c$emicals into a batc$ process. Le.el measurements can be con.erte' to electrical signals t$at can be use' for control. -$e most common control loop t$at inclu'es le.el measurement is &it$ operation of pumps. 6.2.4.4: Flow Measurement -$e final process .ariable t$at &ill be 'iscusse' is flo& rate. Flo& rate measurement &ill generally only be nee'e' if a continuous flo& process is use'. -$ere are a number of met$o's for measuring flo& rates! but t$e most commonly use' approac$ in c$emical processes are 'ifferential pressure flo& meters an' positi.e 'isplacement flo& meters. Flo& meters can be use' in monitoring an' control. -$e most common control loop t$at inclu'es flo& rate is &it$ operation of pumps. Differential flo& meters measure t$e 'ifference in pressure bet&een t$e t&o si'es of a restriction in a confine' stream. -$ese flo& meters are base' on restrictions impose' by a .enturi tube! an orifice plate or a flo& no;;le &it$ t$e orifice plate meter being t$e most common. -$e orifice plate $ole s$oul' be appropriately si;e' for t$e flo& rate range of interest. 8f t$e $ole is too large t$e resulting pressure c$ange an'! t$erefore! accuracy of t$e flo& measurement &ill be inaccurate. 8n contrast! if t$e $ole is too small! t$e flo& rate measurement is at t$e cost of too $ig$ of a pressure 'rop. >$ile orifice plate meters are typically use' for flo& rate measurement an' subse3uent control! it s$oul' be note' t$at t$e meters 'o $a.e some potential problems. First! t$is type of flo& meter is $ig$ly 'epen'ent on t$e 'ensity an' .iscosity of t$e li3ui'. 6rifice plates can ero'e or $a.e blockage! &$ic$ &ill lea' to inaccurate measurement. -$e pressure taps can become plugge' lea'ing to erroneous flo& .alues. Positi.e 'isplacement flo& meters measure flo& rates using t$e flui' to 'isplace a measuring 'e.ice. 7ost common are rotary 'isplacement flo&meters. 8n t$ese meters! flo& rate is measure' by t$e amount of rotation create' by flo& of t$e flui' past a rotary 'e.ice. (n e,ample of a rotary flo& meter is a .ane0li3ui' flo& meter in &$ic$ a set of .anes mounte' on a rotor &it$ opposing pairs rotate' in a cylin'rical c$amber. -$e o.erall monitor an' control system for a process can be ac$ie.e' by in'i.i'ual monitors an' controllers locate' 'irectly at t$e process. /o&e.er! it is most common in t$e c$emical processes to $a.e a centrali;e' system for monitoring an' controlling. -$is can be rea'ily accommo'ate' for most processes by a P2 base' system. ( number of 'ifferent soft&are options are rea'ily a.ailable for t$ese types of systems.

Fig 13F Turbi)% F(ow ,%t%r

?"

6.2.4.1 Pretreatment of Hig Free Fatt! "cid Feedstocks 7any lo& cost fee'stocks are a.ailable for bio'iesel pro'uction. Anfortunately! many of t$ese fee'stocks contain large amounts of free fatty aci's )FF(s*. (s 'iscusse' else&$ere! t$ese free fatty aci's &ill react &it$ alkali catalysts to pro'uce soaps t$at in$ibit t$e reaction. -$e follo&ing ranges of FF( are commonly foun' in bio'iesel fee'stocksF 9efine' .egetable oils G 0.05 H 2ru'e .egetable oil 0." I 0.5H 9estaurant &aste grease 2 I 5H (nimal fat 5 I "0H -rap grease #0 I 100H Jenerally! &$en t$e FF( le.el is less t$an 1H! an' certainly if it is less t$an 0.5H! t$e FF(s can be ignore'. 2ommon catalyst amounts areF +o'ium $y'ro,i'eF 1H of triglyceri'e &eig$t Potassium $y'ro,i'eF 1H of triglyceri'e &eig$t +o'ium met$o,i'eF 0.25H of triglyceri'es &eig$t +oaps may allo& emulsification t$at causes t$e separation of t$e glycerol an' ester p$ases to be less s$arp. +oap formation also pro'uces &ater t$at can $y'roly;e t$e triglyceri'es an' contribute to t$e formation of more soap. Furt$er! catalyst t$at $as been con.erte' to soap is no longer a.ailable to accelerate t$e reaction. >$en FF( le.els are abo.e 1H! it is possible to a'' e,tra alkali catalyst. -$is allo&s a portion of t$e catalyst to be 'e.ote' to neutrali;ing t$e FF(s by forming soap! &$ile still lea.ing enoug$ to act as t$e reaction catalyst.

+ince it takes one mole of catalyst to neutrali;e one mole of FF(! t$e amounts of a''itional catalyst can be calculate' by t$e follo&ing formulasF +o'ium $y'ro,i'eF KHFF(L)0.1##* M 1 H Potassium $y'ro,i'eF KHFF(L)0.1B5*%0.?6 M 1 H +o'ium met$o,i'eF KHFF(L)0.1B0* M 0.25 H For example, when adding sodium methoxide to a feedstock with 1.5 % FFA, the amount of catalyst would be: )1.5*)0.1B0* M 0.25 H N 0.5# H of t$e triglyceri'es &eig$t

?#

4ote t$at a factor of 0.?6 $as been inclu'e' &it$ t$e potassium $y'ro,i'e calculation to reflect t$at reagent gra'e :6/ is only ?6H pure. 8f ot$er gra'es of catalyst are use'! t$is factor s$oul' be a'@uste' to t$eir actual purity. -$is approac$ to neutrali;ing t$e FF(s &ill sometimes &ork &it$ FF( le.els as $ig$ as 5 I 6H. -$e actual limit can 'epen' on &$et$er ot$er types of emulsifiers are present. 8t is especially important to make sure t$at t$e fee'stock contains no &ater. 20"H FF( may be t$e limit if traces of &ater are present. For fee'stocks &it$ $ig$er amounts of FF(! t$e a''ition of e,tra catalyst may create more problems t$an it sol.es. -$e large amount of soap create' can gel. 8t can also pre.ent t$e separation of t$e glycerol from t$e ester. 7oreo.er! t$is tec$ni3ue con.erts t$e FF(s to a &aste pro'uct &$en t$ey coul' be con.erte' to bio'iesel. >$en &orking &it$ fee'stocks t$at contain 50"0H FF( or e.en $ig$er! it is important to con.ert t$e FF(s to bio'iesel or t$e process yiel' &ill be lo&. -$ere are at least four tec$ni3ues for con.erting t$e FF(s to bio'ieselF 1. En#!matic met odsF -$ese met$o's re3uire e,pensi.e en;ymes but seem to be less affecte' by &ater. (t t$e present time! no one is using t$ese met$o's on a commercial scale. 2. $l!cerol!sisF -$is tec$ni3ue in.ol.es a''ing glycerol to t$e fee'stock an' $eating it to $ig$ temperature )20012*! usually &it$ a catalyst suc$ as ;inc c$lori'e.-$e glycerol reacts &it$ t$e FF(s to form mono0 an' 'iglyceri'es. -$e 'ra&back of glycerolysis is t$e $ig$ temperature an' t$at t$e reaction is relati.ely slo&. (n a'.antage is t$at no met$anol is a''e' 'uring t$e pretreatment so t$at as &ater is forme' by t$e reaction FF( M glycerol O monoglyceri'e M &ater -$e &ater imme'iately .apori;es an' can be .ente' from t$e mi,ture. 3. "cid %atal!sis: -$is tec$ni3ue uses a strong aci' suc$ as sulfuric aci' to cataly;e t$e esterification of t$e FF(s an' t$e transesterification of t$e triglyceri'es. -$e reaction 'oes not pro'uce soaps because no alkali metals are present. -$e esterification reaction of t$e FF(s to alco$ol esters is relati.ely fast! procee'ing substantially to completion in one $our at 6012. /o&e.er! t$e transesterification of t$e triglyceri'es is .ery slo&! taking se.eral 'ays to complete. /eating to 1"012 can greatly accelerate t$e reaction but reaction times &ill still be "00#5 minutes. (not$er problem &it$ aci' catalysis is t$at t$e &ater pro'uction from t$e follo&ing reaction FF( M met$anol O met$yl ester M &ater stays in t$e reaction mi,ture an' ultimately stops t$e reaction! usually &ell before reac$ing completion.

?5

4. "cid catal!sis followed &! alkali catal!sis: -$is approac$ sol.es t$e reaction rate problem by using eac$ tec$ni3ue to accomplis$ t$e process for &$ic$ it is best suite'. +ince aci' catalysis is relati.ely fast for con.erting t$e FF(s to met$yl esters! it is use' as a pretreatment for t$e $ig$ FF( fee'stocks. -$en! &$en t$e FF( le.el $as been re'uce' to 0.5H! or lo&er! an alkali catalyst is a''e' to con.ert t$e triglyceri'es to met$yl esters. -$is process can con.ert $ig$ free fatty aci' fee'stocks 3uickly an' effecti.ely. >ater formation is still a problem 'uring t$e pretreatment p$ase. 6ne approac$ is to simply a'' so muc$ e,cess met$anol 'uring t$e pretreatment t$at t$e &ater pro'uce' is 'ilute' to t$e le.el &$ere it 'oes not limit t$e reaction. 7olar ratios of alco$ol to FF( as $ig$ as #0F1 may be nee'e'. -$e 'isa'.antage of t$is approac$ is t$at more energy is re3uire' to reco.er t$e e,cess met$anol. (not$er approac$ &oul' be to let t$e aci'0cataly;e' esterification procee' as far as it &ill go until it is stoppe' by &ater formation. -$en! boil off t$e alco$ol an' &ater. 8f t$e FF( le.el is still too $ig$! t$en a''itional met$anol an'! if necessary! aci' catalyst can be a''e' to continue t$e reaction. -$is process can be continue' for multiple steps an' &ill potentially use less met$anol t$an t$e pre.ious approac$. (gain! t$e 'isa'.antage is t$e large amount of energy re3uire' by t$e 'istillation process. ( less energy intensi.e approac$ is to let t$e aci'0cataly;e' reaction mi,ture settle. (fter a fe& $ours! a met$anol0&ater mi,ture &ill rise to t$e top an' can be remo.e'. -$en! a''itional met$anol an' aci' can be a''e' to continue t$e reaction. 8t is also possible to use flui's suc$ as glycerol an' et$ylene glycol to &as$ t$e &ater from t$e mi,ture. 6.2.4.2 Procedure for Hig FF" Feedstocks 1. 7easure FF( le.el 2. ('' 2.25 g met$anol an' 0.05 g sulfuric aci' for eac$ gram of free fatty aci' in t$e oil or fat. +ulfuric aci' an' met$anol s$oul' be mi,e' first an' t$en a''e' slo&ly to t$e oil. 3. (gitate for one $our at 6006512. 4. Let mi,ture settle. 7et$anol0&ater mi,ture &ill rise to t$e top. Decant t$e met$anol! &ater! an' sulfuric aci' layer. 5. -ake bottom fraction an' measure ne& FF( le.el. 6. 8f FF( is P 0.5H! return to step 2 &it$ ne& FF( le.el. 8f FF( is G 0.5H! procee' to step 5. 1. ('' an amount of met$anol e3ual to 0.215 , Kgrams of unreacte' triglyceri'esL an' an amount of so'ium met$o,i'e e3ual to K0.25 M )HFF(*0.1B0L%100 , Kgrams of unreacte' triglyceri'esL. 7i, t$e so'ium met$o,i'e &it$ t$e met$anol an' t$en a'' to t$e oil. -$is

?6

correspon's to a 6F1 molar ratio of met$anol to oil for t$e unreacte' triglyceri'es. 8t ignores any met$anol t$at may $a.e carrie' o.er from t$e pretreatment. 3. (gitate for 1 $our at 6012.

6."

6perating Bio0Diesel Plant

-o make bio'iesel fuel efficiently from use' .egetable oils an' animal fats &e $a.e to a.oi' one ma@or problemF soap formation. +oap is forme' 'uring base0cataly;e' transesterification )using lye* &$en so'ium ions combine &it$ free fatty aci's present in use' )an' some .irgin* .egetable oils an' animal fats. -$e soaps 'iminis$ t$e yiel' because t$ey bon' t$e met$yl esters to &ater. -$e bon'e' esters get &as$e' out at t$e &as$ing stage but make &ater separation more 'ifficult an' increase &ater consumption. -$is process takes care of t$e free fatty aci's -$is is a simple proce'ure. -$e first0stage process is not transesterification! but pure an' simple E+-E98F82(-864. Esterification is follo&e' by transesterification! but un'er aci' con'itions itQs muc$ slo&er t$an un'er caustic con'itions an' it &onQt 'o a complete oil0to0met$yl ester con.ersion as t$e reaction is muc$ more e3uilibrium0 sensiti.e. >it$out met$anol reco.ery! t$e alco$ol o.er'ose re3uire' &oul' make t$e price of your fuel @ump! an' e.en &it$ reco.ery it &oul' still be muc$ more e,pensi.e. For t$e first stage youQll form a compoun' out of an aci' an' an alco$ol. -$e alco$ol is still met$anol! but instea' of using lye )so'ium $y'ro,i'e*! t$e 2(-(LR+- in t$is reaction is sulfuric aci' )Sbattery aci'S*. 8t nee's B5H sulfuric aci' )battery aci' is aroun' 50H*. +ulfuric aci' is one of t$e commonest c$emicals on Eart$! @ust like lye. 7ore concentrate' sulfuric aci' 00 B?H an' abo.e 00 costs more! but B5H &orks @ust fine if you follo& t$ese 'irections. 6t$er aci's &onQt &orkF it must be sulfuric aci'. -$e secon' stage uses lye! as usual 00 but it only uses about $alf as muc$ as ot$er met$o's. -$e sulfate ion in t$e sulfuric aci' combines &it$ t$e so'ium ion in t$e lye 'uring t$e secon'0stage reaction to form so'ium sulfate! &$ic$ is a &ater0soluble salt an' is remo.e' in t$e &as$. 4o sulfur remains in t$e bio'iesel fuel pro'uct.

?5

Fig 14: P(a)t Di,%)$io)$

Fig 25: P(a)t !3D 2i%w#

??

Fig 21: P(a)t !Top 6i%w#

6.3.1

E+uip,%)t

For t$e process you re3uire t$e follo&ing e3uipment ( bottom0'raine' reactor .essel of 5.5 liters is best! close' on top. 2irculating pump 0.5 /P for mi,ing. -&o 1.2 :> &as$ing0mac$ine immersion $eaters to $eat t$e mi,ture. ( storage 'rum of 5.5 liters. ( mi,er c$amber of 1.5 liters. Eig$t ball .al.es an' one gate .al.es for circulation process. -$ree funnels for pouring reactors. 6ne fifteen liter &as$ing 'rum. (ir pump to pro'uce bubbles. 6ne fume c$amber )( can &ill suffice* 1.5 liters. 6ne con'ensing container of " liters. +i, feet stainless steel pipe for fitting of 'ifferent c$ambers.

?B

 6.3.2

Elbo&s! -0@oints! +ockets! Ani.ersal @oints an' nipples for fitting purposes. ( 12 D2 motor for stirring.

( si, inc$ stirrer. Fi.e meter of electric &ire for $eaters! motor an' pump. .0%,i*a($

For t$e process &e re3uire t$e follo&ing c$emicals. 5 liter of cru'e oil )Ase' egetable oil*. 1 liter of BBH met$anol )2/"6/*. 5 ml of B5H +ulfuric aci' )/2+6#*. 55 ml of 10H P$osp$oric aci' )/"P6#*. 1.5 liter of 'istille' &ater. 5 ml of Dio,in. 5 ml of -etra $y'ro furan )-/F*. 5 ml of n0$e,ane.

6.3.3 T0% pro*%$$ 1. Filter t$e 5L use' cooking oil first as usual. 2. For a successful reaction t$e oil must be free of &ater. /ere are t&o met$o's of remo.ing t$e &ater contentF )a* +ettling t$e &ater outF -$is met$o' sa.es energy. /eat t$e oil to 60 'eg 2 )1#0 'eg F*! maintain t$e temperature for 15 minutes an' t$en pour t$e oil into a settling tank. Let it settle for at least 2# $ours. 7ake sure you ne.er empty t$e settling .essel more t$an B0H. )b* Boiling t$e &ater offF Less0preferre' met$o' as it uses more energy an' $elps to form more FF(s in t$e oil. /eat t$e oil to 100 'eg 2 )212 'eg F*. (s t$e $eat rises &ater separates out an' falls to t$e bottom 00 'rain it off to a.oi' steam e,plosions. 7aintain t$e temperature until no more steam bubbles rise. First stage B0

". 7easure t$e .olume of oil%fats to be processe' )preferably in liters*. #. /eat t$e oil to "5 'eg 2 )B5 'eg F* 00 make sure t$at all soli' fats are melte'. 5. 7et$anolF use only BBHM pure met$anol. 7easure out t$e met$anol 00 0.0? liters of met$anol for eac$ liter of oil%fats )?H by .olume*. ('' t$e 5.4L met$anol to t$e $eate' oil. 6. 7i, for fi.e minutes 00 t$e mi,ture &ill become murky because of sol.ent c$ange )met$anol is a polar compoun'C oil is strongly non0polarC a suspension &ill form*. 5. For eac$ liter of oil%fats a'' 1 milliliter of B5H sulp$uric aci' )/2+6#*. Ase a gra'uate' eye'ropper! a gra'uate' syringe or a pipette. ('' 57L in abo.e mi,. ?. 7i, gently at L6> rpm )'onQt splas$E* &$ile keeping t$e temperature at "5 'eg 2. -$e rotation of your stirrer s$oul' not e,cee' 500 to 600 rpm 00 spee' is not crucial an' splas$e' oil is a mess to clean. B. 7aintain t$e temperature at "5 'eg 2 for one $our t$en stop $eating. 2ontinue stirring. 10. +tir t$e un$eate' mi,ture for anot$er $our! a total of t&o $ours! t$en stop mi,ing. Let t$e mi,ture sit for at least eig$t $ours! o.ernig$t is better. 11. 8n t$e meantime prepare t$e so'ium met$o,i'eF measure 0.12 litre of met$anol for eac$ litre of oil%fat )12H by .olume* an' &eig$ ".1 grams )up to ".5 grams if purity is in 'oubt* of so'ium lye )so'ium $y'ro,i'e! 4a6/* per litre of oil%fat. 7i, t$e lye into t$e met$anol until t$e lye is completely 'issol.e'. 7i, 0.6L of met$anol T 11.5g of 4a6/. Not%F -$is process uses only about $alf t$e usual amount of lye as t$ere is less fat left to transesterify. Ase BBHM pure so'ium $y'ro,i'e lye. (fter opening t$e container! close it again as 3uickly as possible to pre.ent moisture getting in. >eig$ t$e lye carefully 00 using too muc$ &ill complicate t$e &as$ing process later. 12. (fter settling for eig$t $ours! or t$e ne,t morning! pour $alf of t$e prepare' met$o,i'e into t$e un$eate' mi,ture an' mi, for fi.e minutes. -$is &ill neutrali;e t$e sulp$uric aci' an' boost t$e base catalysis. 8f youQ.e use' soli' fat! it probably soli'ifie' 'uring settling 00 gently melt t$e mi,ture first.. 'econd stage -$is is t$e base0cataly;e' stage.

B1

1". /eat t$e mi,ture to 55 'eg 2 )1"1 'eg F* an' maintain for t$e &$ole reaction. 1#. ('' t$e secon' $alf of t$e prepare' so'ium met$o,i'e to t$e $eate' mi,ture an' start mi,ing at t$e same lo& spee' of not more t$an 500 to 600 rpm. 15. -ptio)a(F 8f your reactor allo&s for it! start 'raining glycerine by0pro'uct from t$e bottom 20025 minutes after t$e start of t$e base stage. )Pump0mi,ing &orks best for t$is 00 &it$ pump or mi,er! turn t$e motor off for a fe& minutes if necessary to allo& t$e glycerine to settle.* 9epeat e.ery 10 minutes 00 take care! t$e glycerine is 3uite $ot an' causticE +et asi'e 00 see step 1?. 16. (ll usersF -ake regular samples in a 1S to 1.5S 'iam. glass container. >atc$ for a stra& yello& colour of t$e ester portion. Jlycerine )bro&n an' sticky* &ill settle at t$e bottom of t$e @ar. >$en t$is colour is reac$e' )usually in 1.502.5 $ours* turn t$e $eat an' mi,er off. 8nstea' of taking out samples to c$eck t$e colour you coul' use translucent brai'e' tubing for t$e pump. 15. (llo& to settle for one $our. 1?. -ptio)a(: For easier &as$ingF Drain off t$e glycerine. 7easure off 25H of t$e total glycerine )inclu'ing pre.iously 'raine' glycerine if you follo&e' step 15* an' mi, &it$ 10 millilitres of 10H p$osp$oric aci' )/"P6#* for eac$ litre of oil%fat processe'. -$e mi,ing can be 'one &it$ a &oo'en spoon in a plastic container. Pour t$e aci'ifie' glycerin back into t$e reactor an' stir for 20 minutes! un$eate'. (llo& to settle for at least si, $ours an' t$en 'rain t$e glycerin fraction completely. (u&&le was ing 8t uses a small air0pump! usually an a3uarium aerator pump &it$ a bubble0stone. >ater is a''e' to t$e bio'iesel in t$e &as$ tank )usually a 3uarter to a $alf as muc$ &ater as bio'iesel*C t$e &ater sinks to t$e bottomC t$ro& in t$e bubble0stone! &$ic$ also sinks to t$e bottom! an' s&itc$ on t$e pump. (ir0bubbles )lots of little bubbles is best* rise t$roug$ t$e &ater an' into t$e bio'iesel! carrying a film of &ater aroun' t$em! &$ic$ &as$es t$e bio'iesel aroun' t$e bubble. >$en it reac$es t$e surface t$e bubble bursts! lea.ing t$e &ater to sink back 'o&n again! &as$ing t$e fuel again. Asually t$ree or four &as$es are use'! eac$ of si, to eig$t $ours! often less for t$e first &as$C &it$ a settling perio' of at least 1 $our bet&een &as$es )some people settle it for muc$ longer*. (fter itQs settle' t$e &ater is remo.e' .ia a bottom0'rain an' replace' &it$ &ater. >as$ing is complete' &$en t$e &ater is clear after settling! &it$ a p/ of 5*.
Fig 22: P(a)t op%ratio)

B2

6.3.4

P(a)t -p%ratio)

Plant operates accor'ing to t$e reaction as follo&s. First &e filter t$e oil by funnel. -$en after $eating &e 'rain t$e &ater from .al.e15 an' t$en close it. (fter 'raining &e open t$e .al.e1 an' .al.e3 an' turn on t$e pump. (fter filling &e turn off t$e pump an' close .al.e1 .al.e3. -urn on t$e reactor $eater. 6pen .al.e 3. 6pen .al.e 68 a'' met$anol an' t$en close it. 6pen .al.e 2 9 3! turn on t$e pump for stirring . 6pen .al.e 5 to a'' +ulfuric (ci' an' close it. 8n t$e mean time prepare t$e mi, of met$anol T 4a6/ in 7et$o,i'e 2$amber. -urn of t$e Pump an' a'' open .al.e 1 to a'' /alf of +o'ium 7et$o,i'e. 2lose .al.e 1 an' +tart t$e pump for furt$er +tirring. -urn off t$e pump T open .al.e 5 an' rest of +o'ium 7et$o,i'e t$en close it. +tart t$e pump for some time an' t$en turn it off.

B"

4o& 'rain Jlycerin form .al.e 11T t$en close it. 2lose .al.e 3 T open .al.e 4! turn on t$e pump to get Bio Diesel in >as$ing 2$amber. -urn off Pump an' a'' mi,ture of &ater T /"P6# for &as$ing. Ase (3uarian pump to pro'uce bubbles in &as$ing 2$amber. 4o& 'rain t$e &ater from .al.e 4! rest &ill be clean Bio Diesel in t$e &as$ing 2$amber.

6.3.5

Pu,p S%(%*tio) Pro*%&ur%

'torage % am&er to Reaction % am&er B#

sing !ernoulli"s #$uation

L%2%( 2 L%2%( 1

P1:; < 612:2g<=1<0p>P2:; < 622<=2<?0( /ere =2@=1>2A 0p>2A< ?0( Pip% L%)gt0 >14 T is circuit fitting contains -&o ball .al.es -&o Elbo&s -&o -0Uoints -&o Diffusers +o t$e total $ea' loss comes out to be ?0(>5.162:64.4<5.162:64.4 ?0(>5.5462 0p>5.1666<5.5462 +ince P>B;0p:555 (n'! B>A6 B>5.551366 elocity can be calculate' from flo& rate &$ic$ &as calculate' from &atc$ an' container apparatus B> 5.54642*/$ B5

elocity comes out to be 6>34.5/t:$%* -$is yiel's $ea' 0p>32.1 ,%t%r Reaction to Reaction

L%2%( 2

L%2%( 1

=2@=1>3.3A Pip% L%)gt0>22.1A P1:; < 612:2g<=1<0p>P2:; < 622<=2<?0( =2@=1> P1:; 0p> ?0( T is circuit contains -&o ball .al.es -o& elbo&s -&o - @oints -&o Diffusers -$is makes $ea' loss e3ual to ?0(>5.5462 0p>5.5462 B>5.54642*/$ elocity comes out to be 6>34.5/t:$%* 0p>32.1, B6

Reactor to (io Diesel

L%2%( 2

L%2%( 1

Pip% L%)gt0>21.2A =2@=1>5.3333 P1:; < 612:2g<=1<0p>P2:; < 622<=2<?0( =2@=1>P1:; 0p> ?0( T is circuit contains -&o ball .al.es -o& elbo&s 6ne - @oint -&o Diffusers

-$is makes $ea' loss e3ual to ?0(>5.5662 0p>5.5662 B>5.5533*/$ 6>34.56/t:$%* 0p>23.63, 'election of Pump 2omparing t$e $ea's of t$e circuit

B5

0pa2>23.63<32.1<32.1:3 0pa2>31.34, Ba2> 2.4 */, 2omparing t$e pump $ea's &it$ pump po&er an' flo& rates >e get a pump po&er of 0.5 /P an' B0H P>5.5 CP

0.5 /P pump at #0 m flo& rate T 2.Bcfm

Fig 23: Pu,p S%(%*tio)

B?