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A method and process of recovering metal values Nmero de publicacin WO2017037625 A1

from waste monolithic ceramic capacitors Tipo de publicacin Solicitud
Nmero de solicitud PCT/IB2016/055189
WO 2017037625 A1 Fecha de publicacin 9 Mar 2017
Fecha de presentacin 31 Ago 2016
RESUMEN Fecha de prioridad 2 Sep 2015
Inventores Nitin Gupta, 4 ms

The present invention relates to the recycling process of electronic waste Solicitante Attero Recycling Pvt. Ltd.
resources to recover metals of value. More particularly, it relates to eco-friendly Exportar cita BiBTeX, EndNote, RefMan
yet efcient hydrometallurgical processes to recover metal values from waste Citas de patentes (2), Otras citas (1), Clasicaciones (16),
monolithic ceramic capacitors. In the proposed method, the source material Eventos legales (1)
such as mother boards having MLCC is pulverized using a ball mill to dislodge Enlaces externos: Patentscope, Espacenet
various components such as monolithic ceramic capacitors (MLCC) to form a
powdery mixture of components. The mixture of components is then sieved.
The MLCC powder of particular size range is then subjected to hydrometallurgical process. The process then transfers the precious metals into solution by leaching
process followed by selective precipitation, purication, cementation and nal recovery of metals.

DESCRIPCIN(El texto procesado por OCR puede contener errores) RECLAMACIONES(El texto procesado por OCR puede contener errores)

A process for recovering metals from waste monolithic ceramic capacitors

"A METHOD AND PROCESS OF RECOVERING METAL VALUES FROM WASTE
comprising the steps of:
MONOLITHIC CERAMIC CAPACITORS"

pulverizing of the waste monolithic ceramic capacitors to obtain particles

FIELD OF THE INVENTION of preferred size;

The present invention relates to the recycling process of electronic waste
resources to recover metals of value. More particularly, it relates to eco-friendly
yet efcient hydrometallurgical processes to recover metal values from waste
monolithic ceramic capacitors.
BACKGROUND OF THE INVENTION
sieving of the pulverized capacitors;
preparing an aqueous slurry of sieved powder obtained in step b);
leaching of the aqueous slurry of step c) with hydrochloric acid and
hydrogen peroxide by agitating it for 4-6 hours at a preferred range of
temperature to obtain a leached slurry;

Rapid technological growth and advancement in the electronics domain led to ltering the leached slurry obtained in step d) through a lter press to
generation of new products and a resulting decrease in the life span of obtain a leached liquor containing metals including alkaline earth metals
electronics. Per a study, more than 50 million tons of e-waste were discarded in and transition metals and a residue containing precious metals including
2009 and 72 million tons are expected to be disposed in 2014 (Ping Jiang et gold, silver, and palladium;
al.). E-waste contains precious and special metals, including gold, silver,
treating the leached liquor of step e) with sulphuric acid for selective
palladium and platinum, titanium, nickel copper as well as potentially toxic
precipitation of Barium as barium sulphate;
substances such as lead, mercury, cadmium and beryllium. Hence, a large
scope for recovering such precious metals that can be reused on their recovery. treating the barium free liquor of step f) with sodium hydroxide solution for
selective precipitation of transition metals at their respective pH ranges;
Recycling of electronics allows for precious and special metals to be recovered,
reduces the environmental impact associated with electronic manufacturing agitating the residue of step e) with aqua regia at a preferred temperature
from raw materials, and ensures that hazardous and toxic substances are range for 3-4 hours to obtain a silver rich precipitate and a supernatant
handled properly. Hydrometallurgical processing is emerging as a potential containing gold and palladium;
domestic solution for treating e-waste due to its nontoxic process.
treating the supernatant of step h) with urea and sodium metabisulphite
and ltering the solution to obtain a palladium containing liquor and gold
The study of technologies for the recovery of raw materials from waste
precipitate;
electronic components is therefore of great interest, in terms of environment
protection and reuse of precious raw materials especially metals having a high cementing the palladium from the liquor of step i) with zinc dust and
commercial value. Hydrometallurgy technique is used for obtaining metals from treating the cemented palladium with aqua regia and sodium formate at a
their ores and divided into three general steps viz. leaching, solution preferred range of temperature to obtain palladium powder; and k) melting
concentration
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techniques, on the other hand, are generally performed at temperatures close to the palladium powder of step j) at a temperature ranging from 1200- 1800
ambient temperature, with lower costs and limited atmospheric emissions. C to obtain pure palladium.

Recycling of electronic waste can be divided into mechanical and physical

separation, crushing, enrichment and purication of several stages. Usually the
2. The process of recovering valuable metals as claimed in claim 1, wherein the
rst electronic waste batteries, capacitors, resistors and other major
preferred size of particles is less than 300 .
components of the demolition to remove, and then broken into pieces its pre-
inch size, and then fragments into the grinder pulverized powder pulverized
available pyrometallurgical, hydrometallurgical, electrochemical method further
enrichment, separation. 3. The process of recovering valuable metals as claimed in claim 1, wherein the
preferred range of temperature for leaching of slurry is from 70 to 80 C.

Pyrometallurgical include incineration, plasma furnace and blast furnace

smelting, slag, sinter melting, sweating and high temperature gas-phase
reactions. The basic principle is to use high-temperature metallurgical furnace 4. The process of recovering valuable metals as claimed in claim 1, wherein the
heating stripped nonmetallic materials, precious metal is an alloy with other preferred range of temperature for agitating of residue is from 75 to 95 C.
metals was out of state, re-rening or electrolytic process.

The main steps of hydrometallurgical process includes a series of pickling or

5. The process of recovering valuable metals as claimed in claim 1, wherein the
alkali leaching to separate the solid material, and then subjecting the solution
preferred range of temperature for treating cemented Palladium is from 90 to
such as extraction solution, precipitation, cementation, ion exchange,
100 C.
distillation, ltration and separation processes to separate and enrichment of
some important metals.

Monolithic ceramic capacitors in the e-waste have a good amount of precious 6. The process of recovering valuable metals as claimed in claim 1, wherein the

metals like palladium as well as silver or nickel & tin and the like. There is a preferred range of temperature for melting the Palladium powder is from 1500-

scope to recover and reuse such precious metals from the e-waste that is 1600 C.

scrapped. Hence, an effective approach is needed which is economic and can

effectively recover metals from the e-waste. OBJECT OF THE INVENTION
7. The process of recovering valuable metals as claimed in claim 1, wherein the
The main object of the present invention is to provide a method of recovery transition metals are titanium, copper, nickel, zinc, iron, manganese, and
metal values from waste monolithic ceramic capacitors. chromium.

Yet another object of the present invention is to provide a method of recovering

metals by hydrometallurgical process. 8. The process of recovering valuable metals as claimed in claim 1, wherein the
precipitate of step h) is roasted at a temperature ranging from 550-650 C for 2-
Yet another object of the present invention is to provide an improved method to 4 hours.
separate out precious metal values using selective leaching process.

Yet another object of the present invention is to provide a convenient and eco-
9. The process of recovering precious metals as claimed in claim 9, wherein the
friendly approach for e-waste management. Yet another object of the present
roasted precipitate is agitated with a mixture of nitric acid and water at a
invention is to provide a method wherein the metals are selectively precipitated
temperature ranging from 75-85 C for 1-3 hours and ltered to obtain resid and
and separated from chloride medium using sodium hydroxide solution.
silver rich ltrate.

Yet another object of the present invention is to provide a method for recovering
precious metals including Barium, Titanium, Tin, Copper, Nickel, Gold, Palladium
and Silver and other metals present in e-wastes. 10. The process of recovering precious metals as claimed in claim 10, wherein
the silver is precipitated as silver chloride by treating the ltrate with sodium
chloride solution.
Yet another object of the present invention it to provide a metal recovery
process ends with minimum solid waste and with no liquid discharge.

Yet another object of the present invention is to provide an efcient metal The process of recovering precious metals as claimed in claim 1, wherein the
recovery method with high extraction rate of metal values. precipitation efciency of Barium is 99 %.

SUMMARY OF THE INVENTION

12. The process of recovering precious metals as claimed in claim 1, wherein
The present invention relates to an improved method of recovering metal values the gold precipitate is puried using state of the art process.
from waste monolithic ceramic capacitors. The invention extracts metals in
waste monolithic ceramic capacitors (MLCC) rendered as e-waste. The method

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 is specic to waste MLCC especially from mother boards of computers, laptops and in other MLCC based electronic
equipments.

In the most preferred embodiment of the invention, an improved hydrometallurgical method is provided to segregate
valuable metal from all kind of waste Monolithic ceramic capacitors (MLCC). In this method, the source material such as
mother boards having MLCC is pulverized using a ball mill to dislodge various components such as monolithic ceramic
capacitors (MLCC) to form a powdery mixture of components. The mixture of components is then sieved using a sieve
having pore size of 300 microns. The MLCC powder of below 300 microns is then subjected to hydrometallurgical process.
The process then transfers the precious metals into solution by leaching process followed by selective precipitation,
purication, cementation and nal recovery of metals.

BRIEF DESCRIPTION OF THE DRAWINGS

Figure 1 elucidates the process ow-chart for recovering of total metal values from waste MLCCs.

DETAILED DESCRIPTION OF THE INVENTION

Reference will now be made in detail to the present embodiment of the present invention, by way of accompanying
drawings and claims, examples of which are illustrated in the description below. The embodiments are described below in
order to explain the present invention.

In an embodiment of the invention, an improved hydrometallurgical method is provided to separate out metal values from
all kind of waste Monolithic ceramic capacitors (MLCC). In this method, the source material is pulverized using a size
reduction apparatus preferably a ball mill to liberate the scrap monolithic ceramic capacitors (MLCC) in the form of a
mechanical mixture of particles. The mixture of particles is then sieved using a sieve having pore size of 300 microns. The
MLCC powder of below 300 microns is then subjected to hydrometallurgical process. The process then transfers the
precious metals into solution by leaching process followed by selective precipitation, purication, cementation and nal
recovery of metals.

In another embodiment, as described in Fig. 1, the invention provides a process of metal recovery and comprises the
following steps of: a. Pulverization of Waste monolithic ceramic capacitor (MLCC) using a ball mill. b. Sieving of pulverized
MLCC obtained in step a. with mesh of pore size 300 microns.

c. Primary leaching of MLCC powder of below 300 microns size obtained in step b. with HCI/H202 for metal values other
than precious metals.

d. Leaching of gold and palladium from the above residue of the step c. with aquaregia.

e. Leaching of silver from the above residue of step d. after drying and roasting with Nitric acid.

f. Selective Precipitation of each metal with pH variation using sodium hydroxide solution (except barium which is
precipitated with Sulphuric acid as barium sulphate).

g. Precipitation of Gold from the leach liquor of step d. with Urea and sodium metabisulphite.

h. Cementation of Pd from the above gold free liquor of step g. with zinc dust. i. Purication of Pd by leaching with aqua
regia followed by precipitation with sodium formate.

j. Precipitation of silver from the leach liquor of step e. with sodium chloride, k. Recovery of Cu from Pulverized MLCC of
above 300 microns size of step b., by Electro rening method. In preferred embodiment of the present invention, the waste
MLCC scrap is initially crushed by any crusher, preferably a ball mill. Sieving is then carried out using a sieve of pore size
300 . The MLCC powder having size less than 300 is then subjected to primary leaching process using hydrogen
chloride and hydrogen peroxide solution. The purpose of such a primary leaching is to extract non precious metals of
value. The precious metals remain in form of residue.

Selective leaching for the metals like gold, palladium, silver is then carried out from the residue obtained from primary
leaching process. Gold and palladium are leached out using Aqua Regia. Leaching of silver is then carried out from residue
of step d. after drying and roasting with Nitric acid. Once leaching process is done, each metal is selectively precipitated
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of precipitant(s) for
 selective precipitation process depends upon the metal to be precipitated. For example, barium is precipitated with
sulphuric acid and barium sulphate; gold is precipitated with urea and sodium metabisulphite; silver is precipitated with
sodium chloride. Palladium is cemented from the above gold free liquor with zinc dust.

In another embodiment of the invention, leaching process is provided primarily to leach out precious metals from other
non-precious ones and then series of selective leaching steps take place depending on the type of metal to be leached.
The method provides an economical and eco-friendly approach for e-waste management in the form of metal recovery
from waste MLCC.

The method also provides selective precipitation approach to precipitate out precious metals including Barium, Titanium,
Tin, Copper, Nickel, Gold, Palladium and Silver and other metals abundant in waste MLCC.

In an embodiment of the invention, the method provides an efcient method leaving minimum solid and no liquid wastes
after completion of the recovery process. The average recovery of metallic fraction containing precious metals into basic
concentrate using this method is above 90 % and which is effective.

In principal, the present invention provides for a process for recovering metals from waste monolithic ceramic capacitors
comprising the steps of: a) pulverizing of the waste monolithic ceramic capacitors to obtain particles of preferred size;

b) sieving of the pulverized capacitors;

c) preparing an aqueous slurry of sieved powder obtained in step b);

d) leaching of the aqueous slurry of step c) with hydrochloric acid and hydrogen peroxide by agitating it for 4-6 hours at a
preferred range of temperature to obtain a leached slurry;

e) ltering the leached slurry obtained in step d) through a lter press to obtain a leached liquor containing metals
including alkaline earth metals and transition metals and a residue containing precious metals including gold, silver, and
palladium;

f) treating the leached liquor of step e) with sulphuric acid for selective precipitation of Barium as barium sulphate;

g) treating the barium free liquor of step f) with sodium hydroxide solution for selective precipitation of transition metals at
their respective pH ranges;

h) agitating the residue of step e) with aqua regia at a preferred temperature range for 3-4 hours to obtain a silver rich
precipitate and a supernatant containing gold and palladium;

i) treating the supernatant of step h) with urea and sodium metabisulphite and ltering the solution to obtain a palladium
containing liquor and gold precipitate; j) cementing the palladium from the liquor of step i) with zinc dust and treating the
cemented palladium with aqua regia and sodium formate at a preferred range of temperature to obtain palladium powder;
k) melting the palladium powder of step j) at a temperature ranging from 1200- 1800 C to obtain pure palladium.

The invention will now be illustrated by the following non-limiting examples. Example 1: In a 10 kg batch of waste
monolithic ceramic capacitors, the process was performed. Initially, the sample was pulverized in a ball mill containing
eight iron balls weighing each 18 kg for 6 hours at a speed of 40 rpm and nally sieved to obtain a particle size of less than
300 (8.07 Kg). The chemical analysis of the sieved material is shown in table 1.

Table 1 Chemical analysis of the sieved MLCC

About 2 Kg sample of the sieved material was taken for the study in different batches. Slurry is made by dissolving the
sample in water (about 10 liters). The slurry is then used for primary leaching with hydrochloric acid (about 5.4 liters) and
50% w/v hydrogen peroxide (about 132 ml). The mixture is agitated for ve hours at a temperature ranging from 70 to

80 C. After predetermined time, the slurry was ltered to obtain leach liquor, LA (about 15.9 liters) and residue, RA (about
0.54 Kg). The analysis of the leach liquor, LA is represented in table 2. The leach liquor, LA was taken for selective
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 precipitation of metals. Whereas, the residue, RA was taken for recovering precious metals like gold, silver, and palladium.

Table 2. Chemical analysis of the leach liquor, LA

Elements Cu Ni Zn Sn Fe Ba Al Mn Cr Ti g/l 3.24 12.75 0.41 4.40 4.63 21.00 0.19 0.19 0.38 32.75 The leach liquor, LA was
taken for selective precipitation of metals including alkaline earth metals and transition metals present in the liquor. To
recover alkaline earth metals, leach liquor, LA is treated with sulphuric acid at room temperature (253) C. The treatment
of LA with sulphuric acid (1.6 time stoichiometric amount of Ba in the liquor) results into precipitation of barium as barium
sulphate. More than 99% precipitation efciency was observed and about 0.569 Kg of barium sulphate was collected with
97.8% purity.

In the subsequent step, barium free liquor was taken for recovery of remaining metals that includes transition metals
along with other metals. The barium free liquor is treated with sodium hydroxide at a temperature of 90 C and a pH of 0.5
for atleast 3 hours. The slurry was then ltered to separate residue containing titanium and co-precipitated amounts of tin
(16.5%). More than 98.2% precipitation efciency (for titanium) was observed.

In order to get a pure titanium dioxide, the residue was re-dissolved and re-precipitated at a temperature of 90 C and a pH
of 0.5 for 3 hours. The slurry was ltered, washed and dried at 110 C for 2 hours. Titanium oxide (0.201 Kg) having purity
of 97.9% was collected. The titanium free liquor was taken for the recovery of tin. Tin (Sn) was precipitated using sodium
hydroxide solution (pH 1.2) at room temperature (253) C for 2 hours. The precipitated tin hydroxide was ltered, washed
and dried at 110 C for 2 hours. About 0.076 Kg of tin oxide was collected with a purity of 98.8%.

I n the subsequent study, the impurities including iron, aluminium, zinc and chromium was removed using sodium
hydroxide solution (pH 4.5). After removing impurities, copper and nickel were recovered using sodium hydroxide solution
at a pH of 5.5 and 9 respectively. About 0.076 Kg of copper hydroxide and 0.32 Kg of nickel hydroxide were recovered.

Recovery of precious metals: For recovering precious metals, the residue, RA (0.54 Kg) was taken and agitated with about
1.25 liters of aqua regia at a temperature of 80 C for 4 hours, to leach out precious metals. The slurry was then cooled,
ltered and washed. The residue, RB (about 0.48 Kg) and leach liquor, LB (about 2.8 liters) were collected. Leach liquor, LB
was taken for precipitation of gold and palladium, while the residue, RB was taken for silver (Ag) recovery. The chemical
analysis of the leach liquor, LB is presented in Table 3. More than 90% leaching efciency of both gold (Au) and palladium
(Pd) was observed.

Table 3. Chemical analysis of aqua regia leach liquor-2

Recovery of Gold (Au) and palladium (Pd): About 0.3 Kg of urea was added to the leach liquor, LB and agitated. The gold
(Au) was precipitated by adding 0.5 g of sodium metabisulphite. The precipitated gold was taken out by ltration followed
by washing and drying. The dry weight of gold powder was found to be 0.29 g.

The gold free ltrate was taken for palladium recovery. I nitially, palladium was cemented by using zinc dust at a
concentration of 8 g/L, the cemented palladium was re-dissolved in aqua regia and re-precipitated using sodium formate
at a concentration of 22 g/L and a temperature, 95 C. The precipitated palladium was ltered, washed and dried and
nally melted at 1600 C. The weight of palladium metal was 0.75 g.

The residue, RB was roasted at 600 C for three hours. The roasted residue was agitated with nitric acid (0.4 liter) and
water (1.0 liter) at 80 C for 2 hours. The slurry was ltered, washed and dried at 110 C for two hours. The weight of the
nal residue was found to be 0.32 Kg. To the ltrate (1.28 liter), saturated sodium chloride solution was added till the
complete precipitation of silver. The precipitated silver chloride was washed, dried and melted at 1000 C. The weight of
silver metal obtained was 14 g. The chemical analysis of the nal residue was presented in Table 4. Table 4: Chemical
analysis of the nal residue

Example-2: Another batch of 2 Kg sieved sample was taken for the study. Slurry is made by dissolving the sample in water
(about 10 liters). The slurry is then used for primary leaching with hydrochloric acid (about 5.4 liters) and 50% w/v
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The mixture is agitated for ve hours at a temperature ranging from 70 to 80 C. After predetermined time, the slurry was
ltered to obtain leach liquor, L2A (about 15.7 liters) and residue, R2A (about 0.52 Kg). The analysis of the leach liquor, L2A
is represented in table 2. The leach liquor was taken for selective precipitation of metals present in the leach liquor.
Whereas, the residue, R2A was taken for recovering precious metals like gold, silver, and palladium.

Table la Chemical analysis of the leach liq uor, L.2A

The leach liquor, L2A was taken for selective precipitation of metals. From the leach liquor (L2A), barium was recovered as
barium sulphate by treating with sulphuric acid (1.6 time stoichiometric amount of Ba in the liquor) at room temperature
(253) C. More than 99% precipitation efciency was observed and about 0.565 Kg of barium sulphate was collected with
97.8% purity.

In the subsequent step, barium free liquor was treated with sodium hydroxide solution at 90 C and a pH of 0.5 for atleast
3 hours. The slurry was then ltered to separate residue containing titanium and co-precipitated amounts of tin (16.5%).
More than 98.2% precipitation efciency (for titanium) was observed. In order to get a pure titanium dioxide, the residue
was re-dissolved and re-precipitated at a temperature of 90 C and a pH of 0.5 for 3 hours. The slurry was ltered, washed
and dried at 110 C for 2 hours. Titanium oxide (0.203 Kg) having purity of 97.9% was collected. The titanium free liquor
was taken for the recovery of tin. Tin (Sn) was precipitated using sodium hydroxide solution (pH 1.2) at room temperature
(253) C for 2 hours. The precipitated tin hydroxide was ltered, washed and dried at 110 C for 2 hours. About 0.09 Kg of
tin oxide was collected with a purity of 98.8%.

I n the subsequent study, the impurities including iron, aluminium, zinc and chromium was removed using sodium
hydroxide solution (pH 4.5). After removing impurities, copper and nickel were recovered using sodium hydroxide solution
at a pH of 5.5 and 9 respectively.

About 0.079 Kg of copper hydroxide and 0.32 Kg of nickel hydroxide were recovered.

Recovery of precious metals: For recovering precious metals, the residue, R2A (0.52 Kg) was taken and agitated with about
1.25 liters of aqua regia at a temperature of 80 C for 4 hours, to leach out precious metals. The slurry was then cooled,
ltered and washed. The residue, R2B (about 0.45 Kg) and leach liquor, L2B (about 2.7 liters) were collected.

Leach liquor, L2B was taken for precipitation of gold and palladium, while the residue, R2B was taken for silver (Ag)
recovery. The chemical analysis of the leach liquor, L2B is presented in Table 2a. More than 90% leaching efciency of both
gold (Au) and palladium (Pd) was observed.

Table 2a: Chemical analysis of aqua regia leach liq uor, L

Recovery of Gold (Au) and palladium (Pd): About 0.312 Kg of urea was added to the leach liquor, L2B and agitated. The
gold (Au) was precipitated by adding 0.5 g of sodium metabisulphite. The precipitated gold was taken out by ltration
followed by washing and drying. The dry weight of gold powder was found to be 0.29 g.

The gold free ltrate was taken for palladium recovery. I nitially, palladium was cemented by using zinc dust at a
concentration of 8 g/L, the cemented palladium was re-dissolved in aqua regia and re-precipitated using sodium formate
at a concentration of 22 g/L and a temperature, 95 C. The precipitated palladium was ltered, washed and dried and
nally melted at 1600 C. The weight of palladium metal was 0.78 g.

The residue, R2B was roasted at 600 C for three hours. The roasted residue was agitated with nitric acid (0.4 liter) and
water (1.0 liter) at 80 C for 2 hours. The slurry was ltered, washed and dried at 110 C for two hours. The weight of the
nal residue was found to be 0.31 Kg. To the ltrate (1.26 liter), saturated sodium chloride solution was added till the
complete precipitation of silver. The precipitated silver chloride was washed, dried and melted at 1000 C. The weight of
silver metal obtained was 14.3 g. The chemical analysis of the nal residue was presented in Table 3a.

Table 3a. Chemical analysis of the nal residue

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Elements Cu Ni Pb Zn Au Ag Pd Sn Fe Al Mn Cr Ba Ti

% BDL BDL BDL BDL 0.003 0.16 0.006 BDL BDL BDL BDL BDL BDL BDL

CITAS DE PATENTES
Patente citada Fecha de presentacin Fecha de publicacin Solicitante Ttulo
Advanced
Sustainable process for reclaiming precious metals and
WO2012024603A2 * 19 Ago 2011 23 Feb 2012 Technology
base metals from e-waste
Materials, Inc.
Advanced
Apparatus and method for stripping solder metals during
WO2013090517A1 * 13 Dic 2012 20 Jun 2013 Technology
the recycling of waste electrical and electronic equipment
Materials, Inc.
* Citada por examinador

OTRAS CITAS
Referencia
1 None

CLASIFICACIONES

Clasicacin
C22B3/00, C22B25/06, C22B7/00, C22B26/20, C22B15/00, C22B34/12
internacional
Y02P10/228, Y02P10/236, Y02P10/234, Y02P10/214, C22B11/046, C22B7/007, C22B26/20, C22B34/12, C22B25/06,
Clasicacin cooperativa
C22B15/0067

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