CN109626411A - A kind of production technology of anhydrous stannous chloride - Google Patents
A kind of production technology of anhydrous stannous chloride Download PDFInfo
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- CN109626411A CN109626411A CN201710931944.4A CN201710931944A CN109626411A CN 109626411 A CN109626411 A CN 109626411A CN 201710931944 A CN201710931944 A CN 201710931944A CN 109626411 A CN109626411 A CN 109626411A
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- stannous chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/04—Halides
- C01G3/05—Chlorides
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of production technologies of anhydrous stannous chloride, include the following steps: a, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity;B, it is removed into step a in the etching solution of impurity and enough sodium hydroxide solutions is added;C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly;D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating;E, after taking out the stannous chloride generated in step d precipitating, pure water rinse is used;F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after being rinsed in step e, obtain anhydrous stannous chloride.It is low using the anhydrous stannous chloride purity is high of this method preparation, impurity content, and the pollution to air environment is reduced, improve working environment.
Description
Technical field
The present invention relates to environmental protective chemical industry technical fields, more specifically, it relates to a kind of production work of anhydrous stannous chloride
Skill.
Background technique
In recent years, China's electronic product industry is quickly grown, especially smart phone, tablet computer, laptop
Sales volume rapid development.Printed wiring board is the Main electronic parts in electronic product, can be generated during printed wiring board big
The etching solution of amount, the main component in printed circuit board etching waste liquor is copper chloride and hydrochloric acid, utilizes the copper chloride in etching solution
High-purity stannous chloride is prepared, is had high economic benefit.
A kind of useless copper chloride fluid of etching board production chlorine of utilization is disclosed in the Chinese invention patent that notification number is CN1105341
Change cuprous method, displace copper powder with useless acidic copper chloride fluid of etching board and scrap iron reaction first, then by made copper powder and spent acid
Property copper chloride fluid of etching board and chloride complexing agent be uniformly mixed, heat and keep the temperature a period of time, generate cuprous chloride complexation object;It is past
Add water in the complex solution, hydrolyze the complex compound, generates white stannous chloride precipitating;Stannous chloride is precipitated decompression to take out
After filter, dried after hydrochloric acid and ethyl alcohol wash respectively, then sealed package.
Stannous chloride content made from above-mentioned preparation method is only 96.5%, and the high-copper salt content in impurity is up to 2%,
And since which introduce iron powders, iron tramp is inevitably introduced, is easy to cause iron tramp exceeded.It is, therefore, desirable to provide
A kind of new scheme solves the above problems.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of production work of anhydrous stannous chloride
Skill has the advantages that anhydrous stannous chloride purity is high, impurity content are low.
To achieve the above object, the present invention provides the following technical scheme that
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity;
B, it is removed into step a in the etching solution of impurity and enough sodium hydroxide solutions is added;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating;
E, after taking out the stannous chloride generated in step d precipitating, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after being rinsed in step e, obtain anhydrous stannous chloride.
By adopting the above technical scheme, since etching liquid acidity is higher, pH is up to 0-1, by the way that hydrogen-oxygen is added in etching solution
Change sodium, improve the pH value of etching solution, while the copper chloride in etching solution and sodium hydroxide generate Kocide SD precipitating, improve solution
PH is conducive to the precipitation of Kocide SD precipitating.It hydrochloric acid in etching solution and the Kocide SD precipitating generated and is newly added
Kocide SD generate copper chloride, Kocide SD is added in etching solution, on the one hand increases the concentration of copper chloride, on the other hand into
One step improves the pH of solution, consumes the hydrochloric acid in etching solution.The amount for reducing the sodium sulfite of hydrochloric acid consumption, improves stannous chloride
Yield.Due to being not introduced into other heteroions in reaction, sodium ion can be removed by pure water rinse and water absorbing agent drying, from
And the purity of anhydrous stannous chloride is improved, reduce impurity content.
Due to being exothermic reaction when sodium sulfite is reacted with copper chloride generates stannous chloride, the heat of releasing can accelerate it
The rate that the reaction was continued, and do not need to heat, save the energy.
Further preferably are as follows: it is 6-6.8 that pH is controlled in the step c.
By adopting the above technical scheme, keep etching solution weakly acidic, Kocide SD precipitating and the hydrochloric acid in etching solution of addition
Fully reacting avoids that excessive Kocide SD precipitating is added, reduces the content of the high-copper salt impurity in anhydrous stannous chloride.
Further preferably are as follows: reaction temperature is 38-43 DEG C in the step d.
By adopting the above technical scheme, being reacted due to sodium sulfite with copper chloride when generating stannous chloride is exothermic reaction, control
The temperature for making reaction, on the one hand avoids temperature excessively high, causes cuprous ion is heated oxidation occurs and generates copper ion, reduces product
In high-copper salt impurity content;On the other hand the too low reduction reaction rate of temperature is avoided, the production cycle is shortened.
Further preferably are as follows: the mass percent of copper chloride is 7%-8%, etching solution in the etching solution in the step a
PH be 0-1.
By adopting the above technical scheme, the copper chloride content and pH in former reaction solution are controlled, steady production is conducive to, stablizes nothing
The quality of water stannous chloride.
Further preferably are as follows: device for absorbing tail gas is provided on the reaction vessel, the device for absorbing tail gas is provided with
Absorbing liquid, the device for absorbing tail gas are used to remove the sulfur dioxide and hydrogen chloride gas that side reaction generates in step d.
By adopting the above technical scheme, pH value when generating stannous chloride due to reaction is 6.5 or so, so there is side reaction hair
Raw, side reaction is that sodium sulfite reacts the toxic sulfur dioxide gas of generation with hydrochloric acid, can also be distributed after a small amount of hydrochloric acid volatilization
Into air, by device for absorbing tail gas sulfur dioxide absorption and hydrogen chloride gas, the pollution to surrounding air environment is reduced, is changed
Kind working environment.
Further preferably are as follows: the absorbing liquid is the sodium hydroxide solution that mass percent is 20%.
By adopting the above technical scheme, sodium hydroxide is high to the sour gas such as sulfur dioxide and hydrogen chloride absorptivity, reduces ease
Sulfur dioxide and hydrogen chloride into air out reduces the pollution to surrounding air environment, improves working environment.
Further preferably are as follows: water absorbing agent is absolute alcohol or solid alcohol in the step f.
By adopting the above technical scheme, be oxidized easily under dampness due to stannous chloride, using absolute alcohol or
Solid alcohol removes a small amount of water in stannous chloride, improves the purity of stannous chloride.
Further preferably are as follows: it is 3-4 that pH is controlled in the step b.
By adopting the above technical scheme, pH is conducive to the Kocide SD being added dissolution between 3-4, can also be to avoid generation hydrogen
Copper oxide precipitating, reduces the content of high-copper salt impurity in product.
Further preferably are as follows: further include having step g: by the sewage that centrifugal dehydration obtains in rinsing in step e and step f
It is sent into Sewage Disposal processing, detects rear discharge up to standard.
By adopting the above technical scheme, the content of the copper ions in sewage after centrifugal dehydration is less than 1%, due to sufficiently recycling
Copper ion in discarded etching solution, reduces the difficulty and cost of subsequent sewage treatment, energy conservation and environmental protection.
In conclusion the invention has the following advantages: Kocide SD is added in etching solution, by pH and temperature
Control, on the one hand increase the concentration of copper chloride, on the other hand further increase the pH of solution, consume the salt in etching solution
Acid.The amount for reducing the sodium sulfite of hydrochloric acid consumption, improves the yield of stannous chloride.Due to reaction when be not introduced into other it is miscellaneous from
Son, sodium ion can be removed by pure water rinse and alcohol drying, to improve the purity of anhydrous stannous chloride, be reduced
Impurity content.Due to being exothermic reaction when sodium sulfite is reacted with copper chloride generates stannous chloride, the heat of releasing can be accelerated
Its rate that the reaction was continued, and do not need to heat, save the energy.The two of side reaction release are absorbed by device for absorbing tail gas
Sulfur oxide and hydrogen chloride gas reduce the pollution to surrounding air environment, improve working environment.
Specific embodiment
Below with reference to embodiment, the present invention will be described in detail.
Embodiment 1:
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity, stannous chloride in etching solution
Mass percent is 7%, and the pH of etching solution is 0;
B, it is removed into step a and the sodium hydroxide solution that enough mass percents are 30% is added in the etching solution of impurity, made
PH is 3;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly, control
PH processed is 6, and the outlet of reaction vessel is provided with device for absorbing tail gas, and the sodium hydroxide that device for absorbing tail gas is provided with 20% is molten
Liquid;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating, control
Reaction temperature is 38 DEG C, and the gas generated in reaction process is passed through in sodium hydroxide solution by device for absorbing tail gas;
E, after reaction terminating, after the stannous chloride generated in step d precipitating is taken out, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after rinsing in step e, water absorbing agent is absolute alcohol, is obtained
To anhydrous stannous chloride.
Embodiment 2:
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity, stannous chloride in etching solution
Mass percent is 7.2%, and the pH of etching solution is 0.3;
B, it is removed into step a and the sodium hydroxide solution that enough mass percents are 30% is added in the etching solution of impurity, made
PH is 3.2;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly, control
PH processed is 6.2, and the outlet of reaction vessel is provided with device for absorbing tail gas, and the sodium hydroxide that device for absorbing tail gas is provided with 20% is molten
Liquid;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating, control
Reaction temperature is 39 DEG C, and the gas generated in reaction process is passed through in sodium hydroxide solution by device for absorbing tail gas;
E, after reaction terminating, after the stannous chloride generated in step d precipitating is taken out, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after rinsing in step e, water absorbing agent is absolute alcohol, is obtained
To anhydrous stannous chloride.
Embodiment 3:
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity, stannous chloride in etching solution
Mass percent is 7.5%, and the pH of etching solution is 0.5;
B, it is removed into step a and the sodium hydroxide solution that enough mass percents are 30% is added in the etching solution of impurity, made
PH is 3.5;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly, control
PH processed is 6.5, and the outlet of reaction vessel is provided with device for absorbing tail gas, and the sodium hydroxide that device for absorbing tail gas is provided with 20% is molten
Liquid;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating, control
Reaction temperature is 40 DEG C, and the gas generated in reaction process is passed through in sodium hydroxide solution by device for absorbing tail gas;
E, after reaction terminating, after the stannous chloride generated in step d precipitating is taken out, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after rinsing in step e, water absorbing agent is absolute alcohol, is obtained
To anhydrous stannous chloride.
Embodiment 4:
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity, stannous chloride in etching solution
Mass percent is 7.8%, and the pH of etching solution is 0.8;
B, it is removed into step a and the sodium hydroxide solution that enough mass percents are 30% is added in the etching solution of impurity, made
PH is 3.7;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly, control
PH processed is 6.6, and the outlet of reaction vessel is provided with device for absorbing tail gas, and the sodium hydroxide that device for absorbing tail gas is provided with 20% is molten
Liquid;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating, control
Reaction temperature is 41 DEG C, and the gas generated in reaction process is passed through in sodium hydroxide solution by device for absorbing tail gas;
E, after reaction terminating, after the stannous chloride generated in step d precipitating is taken out, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after rinsing in step e, water absorbing agent is absolute alcohol, is obtained
To anhydrous stannous chloride.
Embodiment 5:
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity, stannous chloride in etching solution
Mass percent is 8%, and the pH of etching solution is 1;
B, it is removed into step a and the sodium hydroxide solution that enough mass percents are 30% is added in the etching solution of impurity, made
PH is 4;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly, control
PH processed is 6.8, and the outlet of reaction vessel is provided with device for absorbing tail gas, and the sodium hydroxide that device for absorbing tail gas is provided with 20% is molten
Liquid;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating, control
Reaction temperature is 43 DEG C, and the gas generated in reaction process is passed through in sodium hydroxide solution by device for absorbing tail gas;
E, after reaction terminating, after the stannous chloride generated in step d precipitating is taken out, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after rinsing in step e, water absorbing agent is absolute alcohol, is obtained
To anhydrous stannous chloride.
Embodiment 6:
A kind of production technology of anhydrous stannous chloride, includes the following steps:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity;
B, it is removed into step a in the etching solution of impurity and enough sodium hydroxide solutions is added;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating;
E, after taking out the stannous chloride generated in step d precipitating, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after rinsing in step e, water absorbing agent is anhydrous calcium chloride,
Obtain anhydrous stannous chloride.
Embodiment 7: a kind of production technology of anhydrous stannous chloride, with embodiment 6 the difference is that, the erosion of step a
The mass percent for carving stannous chloride in liquid is 7.5%, and the pH of etching solution is 0.5.
Embodiment 8: a kind of production technology of anhydrous stannous chloride the difference is that, is controlled with embodiment 7 in step b
PH processed is 3.5.
Embodiment 9: a kind of production technology of anhydrous stannous chloride the difference is that, is controlled with embodiment 8 in step c
PH processed is 6.5.
Embodiment 10: a kind of production technology of anhydrous stannous chloride the difference is that, is controlled with embodiment 9 in step d
Reaction temperature processed is 40 DEG C.
Embodiment 11: a kind of production technology of anhydrous stannous chloride, with embodiment 10 the difference is that, in step f
Water absorbing agent is absolute alcohol.
Embodiment 12: a kind of production technology of anhydrous stannous chloride, with embodiment 11 the difference is that, in step f
Water absorbing agent is solid alcohol.
Embodiment 13: a kind of production technology of anhydrous stannous chloride, with embodiment 12 the difference is that, in step c
The outlet of reaction vessel is provided with device for absorbing tail gas, and device for absorbing tail gas is provided with 20% sodium hydroxide solution.
Embodiment 14: a kind of production technology of anhydrous stannous chloride the difference is that, further includes having with embodiment 13
Step g: the sewage that centrifugal dehydration obtains in rinsing in step e and step f is sent into Sewage Disposal processing, after detection is up to standard
Discharge.
Embodiment 15: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, the erosion of step a
The mass percent for carving stannous chloride in liquid is 5%.
Embodiment 16: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, the erosion of step a
The pH for carving liquid is 3.
Embodiment 17: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it is controlled in step b
PH processed is 6.
Embodiment 18: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it is controlled in step b
PH processed is 2.
Embodiment 19: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it is controlled in step c
PH processed is 5.
Embodiment 20: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it is controlled in step c
PH processed is 8.
Embodiment 21: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it is controlled in step d
Reaction temperature processed is 25 DEG C.
Embodiment 22: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it is controlled in step d
Reaction temperature processed is 50 DEG C.
Comparative example 1: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, step b is not added
Enter sodium hydroxide.
Comparative example 2: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, in step c not
Kocide SD is added.
Comparative example 3: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, one in step d
Enough sodium sulfites are added in secondary property, stir evenly.
Comparative example 4: a kind of production technology of anhydrous stannous chloride, difference from example 1 is that, it will be in step e
It is dried under conditions of 100 DEG C after stannous chloride precipitating centrifugal dehydration after rinsing with baking oven, obtains anhydrous stannous chloride.
Test one
Test specimen: using anhydrous stannous chloride obtained in embodiment 1-22 as test specimen 1-22, using comparative example 1-4
Obtained in anhydrous stannous chloride as control sample 1-4, test specimen 1-22 and control sample 1-4 are numbered in order as 1-
26 groups.
Test method: 1-26 group sample is carried out according to method specified in national standard " GB/T 27562-2011 "
Detection.
Test result: the analysis data of the anhydrous stannous chloride of 1-26 group are as shown in table 1.National standard is stannous chloride
(CuCl) content is more than or equal to 96.5%, high mantoquita (CuCl2) content is less than or equal to 2%, as shown in Table 1,23-26 group is anhydrous
The content of stannous chloride is less than national standard, and high mantoquita (CuCl2) content be greater than 2%;And the anhydrous stannous chloride of 1-22 group
Content be all larger than national standard, and high-copper salt content, less than 2%, the content of the especially anhydrous stannous chloride of 1-5 group is up to
99%, and the content of high mantoquita is only 0.21%, illustrates that the production technology of the anhydrous stannous chloride in the application can be improved nothing
The purity of water stannous chloride reduces impurity content, especially reduces the content of high-copper salt impurity.
The analysis data of the 1 anhydrous stannous chloride of 1-26 group of table
Test two
Test specimen: using anhydrous stannous chloride obtained in embodiment 1-5 as test specimen 1-5, number is 1-5 respectively
Group.
Test method: 1-5 group sample is examined according to method specified in national standard " GB/T 27562-2011 "
It surveys.
Test result: the analysis data of the anhydrous stannous chloride of 1-5 group are as shown in table 2.
The analysis data of the 2 anhydrous stannous chloride of 1-5 group of table
The above is only a preferred embodiment of the present invention, protection scope of the present invention is not limited merely to above-described embodiment,
All technical solutions belonged under thinking of the present invention all belong to the scope of protection of the present invention.It should be pointed out that for the art
For those of ordinary skill, several improvements and modifications without departing from the principles of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of production technology of anhydrous stannous chloride, which comprises the steps of:
A, the etching solution containing copper chloride generated in electronics industry is filtered to remove solid impurity;
B, it is removed into step a in the etching solution of impurity and enough sodium hydroxide solutions is added;
C, enough Kocide SDs are first added in the reaction vessel, adds the etching solution obtained in step b, stirs evenly;
D, a small amount of in the etching solution into step c that sodium sulfite is repeatedly added, it stirs evenly, generates stannous chloride precipitating;
E, after taking out the stannous chloride generated in step d precipitating, pure water rinse is used;
F, dry with water absorbing agent after the stannous chloride precipitating centrifugal dehydration after being rinsed in step e, obtain anhydrous stannous chloride.
2. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that control pH in the step c
For 6-6.8.
3. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that react temperature in the step d
Degree is 38-43 DEG C.
4. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that the etching in the step a
The mass percent of copper chloride is 7%-8% in liquid, and the pH of etching solution is 0-1.
5. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that be arranged on the reaction vessel
There is device for absorbing tail gas, the device for absorbing tail gas is provided with absorbing liquid, and the device for absorbing tail gas is used to remove secondary in step d
React the sulfur dioxide and hydrogen chloride gas generated.
6. the production technology of anhydrous stannous chloride according to claim 5, which is characterized in that the absorbing liquid is quality hundred
Divide the sodium hydroxide solution than being 20%.
7. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that water absorbing agent in the step f
For absolute alcohol or solid alcohol.
8. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that control pH in the step b
For 3-4.
9. the production technology of anhydrous stannous chloride according to claim 1, which is characterized in that further include having step g: will walk
Rinsed in rapid e and step f in the obtained sewage of centrifugal dehydration be sent into Sewage Disposal processing, detect it is up to standard after discharge.
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CN112758958A (en) * | 2020-12-21 | 2021-05-07 | 贵州红星电子材料有限公司 | Method for removing chloride ions in sodium sulfate solution |
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CN112758958A (en) * | 2020-12-21 | 2021-05-07 | 贵州红星电子材料有限公司 | Method for removing chloride ions in sodium sulfate solution |
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Denomination of invention: A production process of anhydrous cuprous chloride Effective date of registration: 20230727 Granted publication date: 20210625 Pledgee: Agricultural Bank of China Limited Shanghai Songjiang Sub-branch Pledgor: SHANGHAI JICHENG ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Registration number: Y2023980050062 |