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27/01/2020 CN103012619B - Quitosana sulfonada / quaternizada solúvel em água e método de preparação dos mesmos - Google Patents

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Quitosana sulfonada / quaternizada solúvel em água e seu método de preparação

Abstrato
CN103012619B
A invenção refere-se a um águasulfossado / quaternizado quitosanados quais a fórmula estrutural é
China
mostrada na especi cação. oáguasulfossado / quaternizado quitosana fornecido pela invenção é
um multifuncional água tratamentoagente que contém simultaneamente um grupo de ácido
sulfônico aniônico e um grupo de amônio quaternário catiônico. Comparado com oquitosana baixar PDF Localizar arte anterio
matéria-prima, as funções do águasulfossado / quaternizado quitosana são aumentados, o Semelhante
águasulfossado / quaternizado quitosana pode ser usado no tratamento de industrial água e
desperdício águapara resolver simultaneamente os problemas de incrustação e multiplicação de
Outras línguas: chinês
micróbios, e o efeito anti-incrustação e esterilização é aprimorado em cerca de 50-60%. Na fórmula
estrutural, n é o grau médio de polimerização en é maior que ou igual a e é menor que ou igual a Inventor: 张惠欣, 朱玉 超, 王枫, 孙 冬雪, 杨婷
200.

Aplicações em todo o mundo

2013 CN

Eventos do aplicativo CN201310010243.9A

11-01-2013 Pedido apresentado por 河北

11-01-2013 Prioridade para CN20131001

2013-04-03 Publicação de CN103012619

08-04-2015 Pedido concedido

08-04-2015 Publicação de CN103012619

Info: Citações de patentes (3), Citações de


Citado por (11), Eventos legais, Documento
Prioridade e aplicativos relacionados

links externos: Espacenet, Dossiê Global, Di

Reivindicações (5)

1. a Águasulfonado / quaternizquitosano solúvel quitosana, a fórmula estrutural que é caracterizada por este material é a seguinte:

Onde n é o grau médio de polimerização e 10≤n≤200.

2. o método de preparação de Águasulfonado / quaternizquitosano solúvel quitosana como reivindicado na reivindicação 1, é caracterizado e compre
etapas:

O primeiro passo, junta-se quitosana no reator, em seguida, diminui a dissolução com a solução de ácido acético que a concentração de massa é de

Segundo passo, adiciona novamente persulfato de amônio sob proteção de nitrogênio, agita e dissolve; Sua proporção material é que a cada 0,40gqu
0,02g ~ 0,05g de persulfato de amônio;

3º passo, então 2-acrilamida-2-metilpropanossulfônico (AMPS) é dissolvido em água, mova-se em funil de pressão constante, sob proteção de nitrog
a gota na solução de reação da etapa, mantenha 40 ° C ~ 80 ° C; Sua proporção é que a cada 0,40gquitosana adiciona AMPS1.02g ~ 2.56g;

4º passo, tudo escorre da continuação traseira e agita 3h ~ 6h;

5º passo, o reagente é resfriado à temperatura ambiente e, com solução reguladora de hidrato de sódio a 5% para neutro, use precipitação com solve
a vácuo, obtém sulfatado quitosana;

6º passo, por água-solúvel para sulfatado quitosana obtido acima, aquecendo em seguida água banho a 60 ° C ~ 85 ° C;

Sétimo passo, depois é adicionado cloreto de cloreto de epoxipropiltrimetil em que, reação 6h ~ 12h; Sua proporção é que cada 0,40g de sulfatoquito
g a 1,14 g de cloreto de epoxipropiltrimetil cloreto;

8º passo, reagiu após a precipitação com acetona do produto e a lavagem, secagem a vácuo, nalmente obtém a sulfonação-n-trimetil descrita quito

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27/01/2020 CN103012619B - Quitosana sulfonada / quaternizada solúvel em água e método de preparação dos mesmos - Google Patents
3. o método de preparação de Águasulfonado / quaternizquitosano solúvel quitosana de acordo com a reivindicação 2, o complemento de solução de
é caracterizado pelo primeiro passo descrito é que a cada 0,40 g quitosana adiciona 20 ml de solução de ácido acético.

4. o método de preparação de Águasulfonado / quaternizquitosano solúvel quitosana como reivindicado na reivindicação 2, o solvente misto que é ca
quinto passo descrito é a razão de volume acetona: as soluções de mistura de etanol = 1: 1.

5. a aplicação de Águasulfonado / quaternizquitosano solúvel quitosana como reivindicado na reivindicação 1, é caracterizado pela inibição de escal
e desperdício água oculação, inibição ou esterilização.

Descrição

Um tipo de Águasulfonado / quaternizquitosano solúvel quitosana e método de preparação

Campo técnico

A presente invenção refere-se à preparação de sulfonação-n-trimetil quitosana cloreto, especi camente quitosana e sulfonato sintetizam sulfatado quitosana p
do enxerto, reaja com sal de amônio quaternário e gere uma espécie de Águasulfonado / quaternizquitosano solúvel quitosana.

Formação técnica

Água é que a produção do ser humano é vivida como recurso, dependendo da existência, e na indústria água e águas residuais tratamento, especialmente refrig
industrial de circulação água sistema e a indústria como campo de petróleo, complexo petroquímico, muitas vezes podem usar o água tratamento agentes com
oculação, inibidor, inibidores de escala, esterilantes. Nos últimos anos, compreendem países desenvolvidos, sem fósforo, facilmente biodegradáveis e amigáv
meio ambiente, são a tendência comum de Água Tratamento Desenvolvimento de produtos químicos.

Quitosana é o produto que a base de quitina desacetilase obtém e é um polissacarídeo alcalino iônico de carga positiva natural, possui boa biocompatibilidade,
molecular é enorme, água insolúvel, é dissolvido apenas em ácido minoritário; portanto, é degradado ou é necessária modi cação

Quitosana- o complexo fosfolipídico tem o caráter de certa atividade antimicrobiana, propriedades formadoras de lme, pode ser um bom germicida anti-séptic
de manutenção de frutas e vegetais, aditivo de alimentos e acabamentos etc. nos alimentos; De acordo com a biocompatibilidade e a degradabilidade
deQuitosanacomplexo fosfolipídico, igualmente no campo dos medicamentos e aplica-se amplamente. Ser intitulado "Métodos sintéticos e aplicações da fraçã
piridilmetil contendo quitosana e seus derivados quaternizados: uma revisão" (WarayuthSajomsang, Carbohydrate Polymers, 2010,80 (3): 631- 647), no docume
alguns métodos de preparação de quitosana sal de amônio quaternário e a propriedade bactericida na medicina biológica é descrita em detalhes. Quitosanapes
complexo fosfolipídico da propriedade bactericida em água tratamento raramente tem relatório.

Quitosanacomplexo fosfolipídico tem certo poder de seqüestro, pode adsorver e quelar resíduos industriais Água Os tratamentos em íons metálicos mantêm a
Ser intitulado "Microondas sintetizam cm-quitosana e propriedades inibidoras de incrustações são estudadas "(Zhang Huixin etc., Tratamento Industrial Água20
(12): 39 ~ 42), no documento, a carboximetilação é realizada para quitosana, utilize a propriedade de absorção de carboxila, hidroxila, quelante de amino, apliqu
Tratamento Industrial Água, mostra a pesquisa, cm-quitosana tem boas propriedades de inibição de incrustações, tendo certa tolerância ao íon cálcio, é um inib
muito promissor da escala verde. Como a comparação de desempenho é única, deve ser usada com outros medicamentos simultaneamente, apenas para ating
objetivo da aplicação, praticamente causar complicações no processo, o consumo de energia também aumenta. .

Em um mundo; Quitosana-fosfolipídeo complexo quase não tem toxicidade; biodegradável; efeito de ação é próximo ao tradicionaláguacondicionador; há uma
investigação e aplicação muito altas que valem a pena; se seu poder de seqüestro e propriedade bactericida forem totalmente utilizados e seu desempenho, pu
efetivamente resolver e os danos que causam a incrustação são controlados no processoágua e crescimento microbiano, para solução água crise de recursos
altamente signi cativa.

Sumario da invenção

O principal objetivo da presente invenção é que a preparação seja um tipo que não apenas contenha grupo sulfônico simultaneamente, mas também compreen
quitosana derivado do grupo quaternário de amônio, produzir produto modi cado Tratamento Industrial Água, desempenhar o efeito da esterilização por inibiçã
escala, ser considerado multifuncional água agente de tratamento, dar o jogo completo ao efeito de multifuncional integrado.Quaternizado modi cado para a s
de quitosana, o desempenho do aplicativo quitosana em processo água e águas residuais tratamento é muito melhorado.

O esquema técnico da presente invenção é:

Um tipo de Águasulfonado / quaternizquitosano solúvel quitosana, sua fórmula estrutural é:

Onde n é o grau médio de polimerização e 10≤n≤200.

O método de preparação descrito Águasulfonado / quaternizquitosano solúvel quitosana, compreende as seguintes etapas:

O primeiro passo, junta-se quitosana no reator, em seguida, diminui a dissolução com a solução de ácido acético que a concentração de massa é de 1%;

Segundo passo, adiciona novamente persulfato de amônio sob proteção de nitrogênio, agita e dissolve; Sua proporção material é que a cada 0,40gquitosana ad
0,02g ~ 0,05g de persulfato de amônio;

3º passo, então 2-acrilamida-2-metilpropanossulfônico (AMPS) é dissolvido em água, mova-se em funil de pressão constante, sob proteção de nitrogênio, junte
a gota na solução de reação da etapa, mantenha 40 ° C ~ 80 ° C; Sua proporção é que a cada 0,40gquitosana adiciona AMPS1.02g ~ 2.56g;

4º passo, tudo escorre da continuação traseira e agita 3h ~ 6h;

5º passo, o reagente é resfriado à temperatura ambiente e, com solução reguladora de hidrato de sódio a 5% para neutro, use precipitação com solvente misto,
a vácuo, obtém sulfatado quitosana;

6º passo, por água-solúvel para sulfatado quitosana obtido acima, aquecendo em seguida água banho a 60 ° C ~ 85 ° C;

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Sétimo passo, depois é adicionado cloreto de cloreto de epoxipropiltrimetil em que, reação 6h ~ 12h; Sua proporção é que cada 0,40g de sulfatoquitosana adici
g a 1,14 g de cloreto de epoxipropiltrimetil cloreto;

8th step, has reacted after product acetone precipitation, and washing, vacuum-drying, nally obtains described sulfonation-n-trimethyl chitosan chloride.

The acetic acid solution add-on of the described the rst step is that every 0.40g chitosan adds 20mL acetic acid solution;

The mixed solvent of the 5th described step is volume ratio acetone: the mixing solutions of ethanol=1:1.

The application of described sulfonation-n-trimethyl chitosan chloride, for the scale inhibition of process water and waste water, occulation, inhibition or germi
treatment.

The present invention has prepared the not only sulfonic group containing scale effect but also the sulfonation-n-trimethyl chitosan chloride of the quaternary am
salt group containing germicidal action, makes chitosan have strong both sexes electrical characteristic and in water treatment, have good application performa

Inhibitor mechanism of the present invention is: (1) complexing solubilising.After Scale inhibitors is water-soluble, the metallic cation in solution can be captured
complexing, improve metal ion solubleness in the solution.(2) dispersion and occulation.Anionic group is adsorbed on fouled surfaces, and colloidal materials
general also with negative charge, can produce repulsive interaction each other, or is surrounded by dirt crystal grain due to adsorption, suppresses grain growin
it be distributed in water.If dirt is formed, because negatively charged ion has the characteristic of polar group, be preferentially adsorbed on dirty layer, by the re
of non-polar group, established dirt rearranged, and then the dirt that disappears.(3) lattice distortion.After Scale inhibitors is added to the water, can chelating s
cations or be adsorbed on dirt surface, destroy or disturb its normal growth, make dirt lattice produce distortion.

Sterilization mechanism of the present invention is: cationic compound can change the permeability of cell walls, the transmission of interference or prevention
substance, also affect the discharge of refuse in cell paste simultaneously, cause the protein denaturization in cell paste, nally play effect that is antibacterial o
microorganisms.

Bene cial effect of the present invention:

The present invention makes full use of resourceful natural product, and being modi edly applied in the middle of water treatment by it, is that a kind of Novel no
harmless, biocompatibility is good, biodegradable Green Water Treatment Reagents.

The present invention has carried out the evaluation of scale-inhibiting properties according to " the mensuration tosca method of GB/T16632-2008 water condi
scale-inhibiting properties " to modi ed product, and scale inhibition performance is 50% ~ 90%; Evaluate the sterilization effect of modi ed product according t
GB/T14643.1-2009 industrial circulating cooling water the measuring method rst part of bacterium algae: mucus forms the mensuration plate count of bacteri
sterilizing rate is more than 90%.

The invention relates to a kind of multifunctional water treating agent simultaneously comprising anion sulfoacid base and cationic quaternary ammonium grou
compared to chitosan raw material, its function increases, industrial water and wastewater treatment can be applied to, solve the problem of fouling and microb
growth, the action effect of scale inhibition and sterilization also improves about 50% ~ 60% simultaneously.

Accompanying drawing explanation

Fig. 1 is the infrared spectra spectrogram of the sulfated chitosan that embodiment 1 obtains;

Fig. 2 is the infrared spectra spectrogram of sulfonation-n-trimethyl chitosan chloride that embodiment 10 obtains;

Fig. 3 is the proton nmr spectra spectrogram of the sulfated chitosan that embodiment 1 obtains;

Fig. 4 is the proton nmr spectra spectrogram of sulfonation-n-trimethyl chitosan chloride that embodiment 10 obtains.

Embodiment

Chitosan (purchased from Jinan Haidebei Marine Organism Engineering Co., Ltd.), be a kind of chain polymer, its structure is:

Wherein, n is mean polymerisation degree, and 10≤n≤200.

A large amount of hydroxyls and amino active group is there is in molecular chain, by 2-acrylamide-2-methyl propane sulfonic (AMPS) and epoxypropyltrimethylc
chloride, modi cation is carried out to it, obtain the sulfonation-n-trimethyl chitosan chloride of said structure in theory, actual experiment data show to have obt
sulfonation-n-trimethyl chitosan chloride equally.

The performance evaluation of the embodiment of the present invention has carried out the evaluation of scale-inhibiting properties according to " the mensurat
method of GB/T16632-2008 water conditioner scale-inhibiting properties " to modi ed product; According to " in GB/T14643.1-2009 industrial circulating cooling
the measuring method rst part of bacterium algae: mucus forms the mensuration plate count of bacterium ", the sterilization effect of modi ed product is evalu

Further illustrate the present invention with embodiment below, embodiment, only for describing the present invention in detail, is not considered as the restrictio
claims in the present invention protection domain.

Embodiment 1:

Take polymerization degree n be the chitosan 0.40g of 30 in reactor, use 20mL1%(w/w) acetic acid solution stirring and dissolving; Add ammonium persulphate
under nitrogen protection, continue to be stirred to ammonium persulphate and dissolve completely; Take AMPS2.05g to dissolve in 20mL water, solution is mov
constant pressure funnel and be assemblied in be placed in 60 DEG C of waters bath with thermostatic control reactor on, under nitrogen protection, AMPS drop
joined in reactor, all drip off rear continuation stir 4h; Reactant is cooled to room temperature, with 5% sodium hydrate regulator solution to neutral, uses mixed s
(acetone: ethanol=1:1, v/v) precipitation, and vacuum-drying, thus obtained sulfated chitosan.When evaluation of anti-scale display n is 30, the scale inhibition
performance of sulfated chitosan is 89%.

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The sign of products therefrom is as follows:

(instrument is the TENSOR27 type FTIR technique instrument that Bruker company produces, light path 400 ~ 4000cm to adopt pellet technique sample prepara
carry out infrared absorption spectrum analysis -1, scan 16 times, resolving power 4cm -1).As seen from Figure 1, at 3444cm -1the absorption peak at place is sh
shows that hydrogen bond disappears, namely on the hydroxyl and amino of chitosan molecule, there occurs derivative reaction.2900cm -1the absorption peak a
right place is the stretching vibration absorption band of alkyl C-H.At 1660cm -1the peak at place is carbonyl absorption peak in AMPS amide group (-NH-CO-).13
-1and 1369cm -1the peak located is that the formation vibration together with methyl in AMPS causes.At 1219cm -1and 1042cm -1the peak at place is sulfonic g

3) charateristic avsorption band, prove that AMPS is grafted on chitosan.

With D 2o has carried out hydrogen nuclear magnetic resonance spectrum analysis (instrument is the Bruker AV400 type superconduction Fourier transform nuc
magnetic resonance spectrometer of Bruker company) as solvent.As seen from Figure 3, the peak about δ=1.50 is the peak of methyl in AMPS; The peak at δ=2
2.40 place is the peak of the methylene radical be connected with amino or hydroxyl in AMPS; Peak near δ=2.80 is the peak of the methyne be connected with ca
The peak of δ=3.00 ~ 4.00 is the hydrogen on chitosan skeleton, proves that AMPS is successfully grafted on chitosan.

From above experimental result and characterization data, chitosan and AMPS react successfully obtained sulfated chitosan with this understanding, and the pe
essential groups is very remarkable, and scale-inhibiting properties is fairly obvious.

Embodiment 2:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 60, and ammonium persulphate is 0.02g, AMPS consum
1.02g, bath temperature 40 DEG C, and the reaction times controls as 3h, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 60, the scale
inhibition performance of sulfated chitosan is 73%.

Embodiment 3:

Step is with embodiment 2, and difference is to take the chitosan 0.40g that polymerization degree n is 180, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 180, the scale inhibition performance of sulfated chitosan is 53%.

Embodiment 4:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 40, and ammonium persulphate is 0.02g, AMPS consum
2.56g, bath temperature 80 DEG C, and the reaction times controls as 6h, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 40, the scale
inhibition performance of sulfated chitosan is 80%.

Embodiment 5:

Step is with embodiment 4, and difference is to take the chitosan 0.40g that polymerization degree n is 120, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 120, the scale inhibition performance of sulfated chitosan is 58%.

Embodiment 6:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 55, and AMPS consumption is 1.02g, and the reaction tim
controls as 3h, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 55, the scale inhibition performance of sulfated chitosan is 78%.

Embodiment 7:

Step is with embodiment 6, and difference is to take the chitosan 0.40g that polymerization degree n is 155, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 155, the scale inhibition performance of sulfated chitosan is 50%.

Embodiment 8:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 44, and bath temperature is set as 80 DEG C, and the rea
times controls as 3h, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 44, the scale inhibition performance of sulfated chitosan is 83%.

Embodiment 9:

Step is with embodiment 8, and difference is to take the chitosan 0.40g that polymerization degree n is 100, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 100, the scale inhibition performance of sulfated chitosan is 58%.

Embodiment 10:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 35, and AMPS consumption is 2.56g, and bath temperatu
as 40 DEG C, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 35, the scale inhibition performance of sulfated chitosan is 87%.

Embodiment 11:

Step is with embodiment 10, and difference is to take the chitosan 0.40g that polymerization degree n is 82, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 82, the scale inhibition performance of sulfated chitosan is 65%.

Embodiment 12:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 46, and ammonium persulphate is 0.05g, AMPS consum
1.02g, and bath temperature is set as 80 DEG C, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 46, the scale inhibition performance o
chitosan is 83%.

Embodiment 13:

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Step is with embodiment 12, and difference is to take the chitosan 0.40g that polymerization degree n is 95, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 95, the scale inhibition performance of sulfated chitosan is 60%.

Embodiment 14:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 38, and ammonium persulphate is 0.05g, bath temperatu
DEG C, and the reaction times controls as 6h, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 38, the scale inhibition performance of s
chitosan is 87%.

Embodiment 15:

Step is with embodiment 14, and difference is to take the chitosan 0.40g that polymerization degree n is 78, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 78, the scale inhibition performance of sulfated chitosan is 66%.

Embodiment 16:

Step is with embodiment 1, and difference is to take the chitosan 0.40g that polymerization degree n is 48, and ammonium persulphate is 0.05g, AMPS consum
2.56g, and the reaction times controls as 3h, thus obtained sulfated chitosan.Evaluation of anti-scale shows: when n is 48, the scale inhibition performance of su
chitosan is 84%.

Embodiment 17:

Step is with embodiment 16, and difference is to take the chitosan 0.40g that polymerization degree n is 105, controls reaction conditions and obtains sulfated
chitosan.Evaluation of anti-scale shows: when n is 105, the scale inhibition performance of sulfated chitosan is 54%.

Embodiment 18:

In 100mL reactor, add the sulfated chitosan 0.40g that n in above-described embodiment 1 is 30, use deionized water dissolving, heating in water bath to 85 DEG
C.Taking 0.76g epoxypropyltrimethylchloride chloride adds wherein, reaction 10h.After reaction terminates, use acetone precipitation, throw out is repeatedly wa
and vacuum-drying, obtained sulfonation-n-trimethyl chitosan chloride.Scale inhibition and sterilization evaluation display: when n is 30, the scale inhibition perfo
of sulfonation-n-trimethyl chitosan chloride is 90%, and sterilizing rate is 99%.

The sign of products therefrom is as follows:

(instrument is the TENSOR27 type FTIR technique instrument that Bruker company produces, light path 400 ~ 4000cm to adopt pellet technique sample prepara
carry out Infrared spectroscopy -1, scan 16 times).As seen from Figure 2, at 1659cm -1the absorption peak at place is carbonyl absorption peak in AMPS amide g
NH-CO-).1386cm -1and 1366cm -1the peak located is that the formation vibration together with methyl in AMPS causes.At 1296cm -1and 1050cm -1the absorptio
at left and right place is sulfonic group (-SO 3) charateristic avsorption band, 1478cm -1be methyl in quaternary ammonium salt, methylene radical absorption pe
that quaternary ammonium salt is grafted to above chitosan.

With D 2o has carried out hydrogen nuclear magnetic resonance spectrum analysis (instrument is the BrukerAV400 type superconduction Fourier transform nuc
magnetic resonance spectrometer of Bruker company) as solvent.As seen from Figure 4, the peak at δ=3.20 place is the peak of methyl in quaternary ammonium
and peak type clearly; The peak at δ=4.20 ~ 4.40 place is the peak of quaternary ammonium salt methylene; The peak of δ=3.00 ~ 4.00 is the hydrogen on chitos
skeleton; The characteristic peak of AMPS still retains, and proves that quaternary ammonium salt is successfully grafted on sulfated chitosan.To sum up phene
analysis, determines the material obtaining structure above.

From above experimental result and characterization data, the characteristic peak of sulfated chitosan still retains, the peak of quaternary ammonium group sig
exists, and proves that sulfated chitosan and epoxypropyltrimethylchloride chloride react successfully obtained sulfonation-n-trimethyl chitosan chloride with th
understanding, scale inhibition and bactericidal property fairly obvious.

Embodiment 19:

Step is with embodiment 18, and difference is to add the sulfated chitosan 0.40g that n is 54, and experimental temperature is heated to 60 DEG C, takes 0.38g
epoxypropyltrimethylchloride chloride and add wherein, the reaction times is 8h, obtained sulfonation-n-trimethyl chitosan chloride.Scale inhibition and sterilizat
evaluation display: when n is 54, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 89%, and sterilizing rate is 96%.

Embodiment 20:

Step is with embodiment 19, and difference is to add the sulfated chitosan 0.40g that n is 175, controls reaction conditions and obtains sulfonation-n-trimethyl c
chloride.Scale inhibition and sterilization evaluation display: when n is 175, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 54%, a
sterilizing rate is 90%.

Embodiment 21:

Step is with embodiment 18, and it is the sulfated chitosan 0.40g of 60 that difference is to add n in above-described embodiment 2, experimental temperature i
to 75 DEG C, takes 0.38g epoxypropyltrimethylchloride chloride and adds wherein, obtained sulfonation-n-trimethyl chitosan chloride.Scale inhibition and steriliz
evaluation display: when n is 60, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 89%, and sterilizing rate is 96%.

Embodiment 22:

Step is with embodiment 21, and difference is to add the sulfated chitosan 0.40g that n is 188, controls reaction conditions and obtains sulfonation-n-trimethyl c
chloride.Scale inhibition and sterilization evaluation display: when n is 188, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 48%, a
sterilizing rate is 90%.

Embodiment 23:

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Step is with embodiment 18, and difference is to add the sulfated chitosan 0.40g that n is 57, and take 0.38g epoxypropyltrimethylchloride chloride and add whe
reaction times is 12h, obtained sulfonation-n-trimethyl chitosan chloride.Scale inhibition and sterilization evaluation display: when n is 57, the scale inhibition
performance of sulfonation-n-trimethyl chitosan chloride is 89%, and sterilizing rate is 96%.

Embodiment 24:

Step is with embodiment 23, and difference is to add the sulfated chitosan 0.40g that n is 170, controls reaction conditions and obtains sulfonation-n-trimethyl c
chloride.Scale inhibition and sterilization evaluation display: when n is 170, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 55%, a
sterilizing rate is 91%.

Embodiment 25:

Step is with embodiment 18, and difference is to add the sulfated chitosan 0.40g that n is 90, and experimental temperature is heated to 75 DEG C, the reaction t
12h, obtained sulfonation-n-trimethyl chitosan chloride.Scale inhibition and sterilization evaluation display: when n is 90, the scale inhibition performance of sulf
n-trimethyl chitosan chloride is 62%, and sterilizing rate is 93%.

Embodiment 26:

Step is with embodiment 18, and difference is to add the sulfated chitosan 0.40g that n is 63, and the reaction times is 8h, obtained sulfonation-n-trimethyl chito
chloride.Scale inhibition and sterilization evaluation display: when n is 63, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 90%, an
sterilizing rate is 96%.

Embodiment 27:

Step is with embodiment 26, and difference is to add the sulfated chitosan 0.40g that n is 118, controls reaction conditions and obtains sulfonation-n-trimethyl c
chloride.Scale inhibition and sterilization evaluation display: when n is 118, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 58%, a
sterilizing rate is 91%.

Embodiment 28:

Step is with embodiment 18, it is the sulfated chitosan 0.40g of 100 that difference is to add n in above-described embodiment 9, experimental temperature is he
60 DEG C, takes 1.14g epoxypropyltrimethylchloride chloride and adds wherein, reaction times is 12h, obtained sulfonation-n-trimethyl chitosan chloride.Scale in
and sterilization evaluation display: when n is 100, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 55%, and sterilizing rate is 92%

Embodiment 29:

Step is with embodiment 28, and difference is to add the sulfated chitosan 0.40g that n is 50, controls reaction conditions and obtains sulfonation-n-trimethyl ch
chloride.Scale inhibition and sterilization evaluation display: when n is 50, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 90%, an
sterilizing rate is 99%.

Embodiment 30:

Step is with embodiment 18, it is the sulfated chitosan 0.40g of 44 that difference is to add n in above-described embodiment 8, experimental temperature is hea
DEG C, takes 1.14g epoxypropyltrimethylchloride chloride and adds wherein, reaction times is 8h, obtained sulfonation-n-trimethyl chitosan chloride.Scale inhibit
sterilization evaluation display: when n is 44, the scale inhibition performance of sulfonation-n-trimethyl chitosan chloride is 90%, and sterilizing rate is 98%.

Embodiment 31:

Step is with embodiment 18, and difference is to add the sulfated chitosan 0.40g that n is 75, takes 1.14g epoxypropyltrimethylchloride chloride and adds where
obtained sulfonation-n-trimethyl chitosan exibição de avaliação de inibição de escala e esterilização: quando n é 75, o desempenho de inibição de escala de sul
n-trimetil quitosana cloreto é de 67% e a taxa de esterilização é de 95%.

A presente invenção não trata de parte e é aplicável à técnica anterior.

Citações de Patentes (3)

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CN103665185A * 2013-09-26 2014-03-26 中国科学院烟台海岸带研 Sulfated chitosan quaternary ammonium salt as well as prep
究所 application thereof

Family To Family Citations

CN103172251B * 2013-04-23 2014-02-12 四川大学 Chitosan-based sludge dewatering occulant and preparation

CN103864231B * 2014-03-11 2015-02-11 山东省泰和水处理有限公 Chitosan multiple-effect water treatment medicine and prepa
司 thereof

CN105770941B * 2014-12-18 2018-04-20 浙江澳兴生物科技有限公 The sterilizing methods of chitosan and chitosan derivatives

CN104817152B * 2015-04-01 2016-08-24 泰祜(上海)石油工程有限 A kind of for occulant processing rejected well drilling liquid
公司 method thereof

CN104987474B * 2015-07-13 2017-07-28 中国科学院新疆理化技术 A kind of preparation method for the magnetic desalination a
研究所 oil eld sewage salinity

CN105176610B * 2015-07-22 2017-09-15 陕西科技大学 A kind of amphoteric chitosan derivative water-coal-slurry ad


preparation method thereof

CN105384263B * 2015-12-07 2018-02-23 湖北地大热能科技有限公 Sulfamic acid modi cation of chitosan water antisludging ag
司 method thereof

CN105367687A * 2015-12-09 2016-03-02 上海大学 Chitosan amphiphilic polymer surfactant, and synthetic meth

CN107903335A * 2017-11-21 2018-04-13 常州可赛成功塑胶材料有 A kind of preparation method of heat-resistance type clay sta
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CN108360071A * 2018-02-25 2018-08-03 温岭汉德高分子科技有限 A kind of etching method of antiradar re ectivity monocrysta
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