CN102746134A - Method for decreasing content of sodium chloride impurities in recovered sodium formate - Google Patents
Method for decreasing content of sodium chloride impurities in recovered sodium formate Download PDFInfo
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- CN102746134A CN102746134A CN2012102429915A CN201210242991A CN102746134A CN 102746134 A CN102746134 A CN 102746134A CN 2012102429915 A CN2012102429915 A CN 2012102429915A CN 201210242991 A CN201210242991 A CN 201210242991A CN 102746134 A CN102746134 A CN 102746134A
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Abstract
The invention relates to a method for decreasing the content of sodium chloride impurities in recovered sodium formate, which is applicable for recovering the sodium formate from a rongalite mother solution. According to the method, sodium chloride is separated out in the concentrating working procedure of a rectified raffinate, and the method comprises the following steps of A. heating the concentrated rectified raffinate to the temperature of 105-110 DEG C under the vacuum degree of -0.08 to -0.09Mpa to separate out the sodium chloride from the raffinate; B. closing the vacuum, emptying, and continuously heating to the temperature of 130-135 DEG C to dissolve the sodium formate which is separated out through crystallization in the vacuum concentrating process of the raffinate; and C. after the temperature reaches to 130-135 DEG C, placing a material into a filter with a jacket, and carrying out vacuum filtration to separate the sodium chloride which is separated out of the material from a material solution; and placing the material solution which is obtained through the filtration into a crystallization kettle, and adding methanol with the volume accounting for about 1/4 of that of the material solution to obtain the recovered sodium formate with the low-content sodium chloride impurities through filter-pressing and drying processes after extraction and crystallization. The content of the sodium formate in a recovered sodium-formate product which is obtained by the method is higher than 88 percent, and the content of the sodium chloride impurities is lower than 5 percent.
Description
Technical field
The present invention relates to a kind of method that reclaims sodium chloride as impurity content in the sodium formiate that reduces, this method is applicable to from the vat powder mother liquor and reclaims sodium formiate.
Technical background
Through the development of nearly two more than ten years, sodium formate method progressively replaces the zinc powder method becomes the topmost method that vat powder is produced.Sodium formiate is one of main raw material of sodium formate method production vat powder; Produce in the process of vat powder at sodium formate method; Generally adopt the excessive technology of sodium formiate, the mother liquor that each reaction produces only some circulation is used for next building-up reactions, and unnecessary mother liquor need comprehensively recycle.Desolventize outside the methyl alcohol in the mother liquor that is processed, also contain inorganic salt such as sodium sulfite anhy 96, Sulfothiorine, sodium formiate, sodium-chlor and the deleterious organic polymer of system.Unnecessary mother liquor comprehensively reclaimed have been become the sodium formate method vat powder at present and has produced requisite technological process.Vat powder is produced unnecessary mother liquor through operations such as neutralization, rectifying, distillation residual liquid concentrate; Obtain sodium sulphite anhydrous 99.3, solvent methanol and recovery sodium formiate respectively, the recovery sodium formiate that wherein obtains at the distillation residual liquid enrichment process returns the vat powder synthesis system as raw materials for production.
Soda ash also is one of main raw material of producing vat powder, and sodium-chlor is the major impurity of soda ash.Reclaim and to come from soda ash on the sodium chloride as impurity source in the sodium formiate and raise with sodium chloride content in the soda ash.When the high recovery sodium formiate of sodium chloride as impurity content returns the vat powder synthesis system as raw materials for production, can cause conversely in the vat powder synthesis mother liquid that sodium chloride content content rises and then the synthetic of vat powder had a negative impact.
Production practice prove; In vat powder mother liquor recycling process; The content of the sodium-chlor in the sodium formiate that the distillation residual liquid enrichment process reclaims is bigger to the influence of vat powder quality product; Sodium chloride content in reclaiming sodium formiate is higher to reach 9% when above, and the vat powder granularity difference of being produced also causes the decline of vat powder product yield.
Although the content of the sodium chloride as impurity in the recovery sodium formiate can be controlled through the sodium chloride content that reduces in the raw material soda ash; But consideration from factors such as reducing production costs; When having to use the higher soda ash of sodium chloride content, then should seek to reduce other approach that reclaims the sodium chloride as impurity content in the sodium formiate.
Summary of the invention
The objective of the invention is to overcome above-mentioned defective, reduce the method that reclaims the sodium chloride as impurity content in the sodium formiate when providing a kind of sodium chloride as impurity content high at raw material soda ash.
Technical scheme of the present invention is: reduce the method that reclaims sodium chloride as impurity content in the sodium formiate; This method is applicable to from the vat powder mother liquor and reclaims sodium formiate; It is characterized in that; The method of sodium chloride as impurity content in the sodium formiate is reclaimed in described reduction, is to isolate sodium-chlor at the distillation residual liquid enrichment process, and process step is following:
A, vacuum tightness-0.08～-0.09Mpa under, it is 105～110 ℃ that heating concentrates distillation residual liquid to temperature of charge, and sodium-chlor is separated out from raffinate;
B, close vacuum, emptying continues to be heated to temperature of charge and reaches 130～135 ℃, makes the sodium formiate dissolving that crystallization is separated out in the raffinate vacuum Concentrating Process;
After C, temperature of charge reach 130～135 ℃, material is put into the strainer with the jacketed of steam heating insulation, vacuum filtration makes the sodium-chlor of separating out in the material separate with material solution;
D, the material solution of suction filtration gained is put into crystallization kettle, add the methyl alcohol of about 1/4 material solution volume, after conventional extraction, crystallization,, obtain the low recovery sodium formiate of sodium chloride as impurity content again through press filtration, drying process.
The recovery sodium formiate product that adopts present method to obtain, its sodium formiate content is greater than 88%, and the impurity sodium chloride content is lower than 5%.
Embodiment
Below with instance the present invention is specified.
Embodiment 1
Certain batch distillation residual liquid between picking up the car, analytical results is: proportion 1.108, sodium-chlor 33.1 grams per liters, S-WAT 2.1 grams per liters, Sulfothiorine 25.3 grams per liters, sodium formiate 197.9 grams per liters.Accumulative total adds 2500 milliliters of above-mentioned distillation residual liquids in 1000 milliliters of four-hole bottles, in vacuum tightness be-0.09Mpa, stir heat down concentrated, when being concentrated into 105 ℃ of solution temperatures; Close vacuum, emptying is when continuing heating and being concentrated into 130 ℃ of solution temperatures; Stop to concentrate, change material over to strainer, vacuum filtration while hot with the jacketed of steam heating insulation; Obtain 410 milliliters of filtratings, this filtrating changing over to is taken back in the crystallization reactor of stream prolong, stirring, adds 100 milliliters methyl alcohol; Natural cooling crystallization to 60～70 ℃, suction filtration, spinning are dried filter cake to such an extent that solid reclaims sodium formiate; Measure the content that reclaims sodium-chlor, S-WAT, Sulfothiorine and sodium formiate in the sodium formiate with chemical analysis, measured value is respectively 4.8%, 1.8%, 3.4% and 89.9%.
Embodiment 2
Accumulative total adds 2500 milliliter the distillation residual liquid identical with embodiment 1 in 1000 milliliters of four-hole bottles, in concentrated vacuum tightness be-0.08Mpa, heat under the stirring concentrated, when being concentrated into 110 ℃ of solution temperatures; Close vacuum, emptying is when continuing heating and being concentrated into 135 ℃ of solution temperatures; Stop to concentrate, change material over to strainer, vacuum filtration while hot with the jacketed of steam heating insulation; Obtain 370 milliliters of filtratings, this filtrating changing over to is taken back in the crystallization reactor of stream prolong, stirring, adds 95 milliliters methyl alcohol; Natural cooling crystallization to 60～70 ℃, suction filtration, spinning are dried filter cake to such an extent that solid reclaims sodium formiate; Measure the content that reclaims sodium-chlor, S-WAT, Sulfothiorine and sodium formiate in the sodium formiate with chemical analysis, measured value is respectively 3.7%, 1.4%, 3.7% and 91.2%.
Embodiment 3
Accumulative total adds the 2500 milliliter distillation residual liquids identical with embodiment 1 in 1000 milliliters of four-hole bottles, in concentrated vacuum tightness be-0.085Mpa, heat under the stirring concentrated, when being concentrated into 108 ℃ of solution temperatures; Close vacuum, emptying is when continuing heating and being concentrated into 132 ℃ of solution temperatures; Stop to concentrate, change material over to strainer, vacuum filtration while hot with the jacketed of steam heating insulation; Obtain 390 milliliters of filtratings, this filtrating changing over to is taken back in the crystallization reactor of stream prolong, stirring, adds 100 milliliters methyl alcohol; Natural cooling crystallization to 60～70 ℃, suction filtration, spinning are dried filter cake to such an extent that solid reclaims sodium formiate; Measure the content that reclaims sodium-chlor, S-WAT, Sulfothiorine and sodium formiate in the sodium formiate with chemical analysis, measured value is respectively 4.3%, 1.7%, 2.5% and 90.5%.
Embodiment 4
On production equipment, use with embodiment 1 identical distillation residual liquid to make an experiment, concentrate vacuum tightness and be-0.09Mpa, when being concentrated into 105 ℃ of solution temperatures; Close vacuum, emptying continues to be heated to 132 ℃; Material is put into the strainer with the jacketed of steam heating insulation, vacuum filtration, filtrating gets in the crystallization reactor of band stirring; The methyl alcohol that adds about 1/4 filtrate volume; Crystallisation by cooling to 60～70 ℃, press filtration, filter cake in vacuum is dry, solid reclaims sodium formiate; Measure the content that reclaims sodium-chlor, S-WAT, Sulfothiorine, fugitive constituent and sodium formiate in the sodium formiate with chemical analysis, measured value is respectively 3.9%, 1.6%, 2.4%, 2.4% and 89.7%.
Claims (1)
1. reduce the method that reclaims sodium chloride as impurity content in the sodium formiate; This method is applicable to from the vat powder mother liquor and reclaims sodium formiate, it is characterized in that, the method for sodium chloride as impurity content in the sodium formiate is reclaimed in described reduction; Be to isolate sodium-chlor at the distillation residual liquid enrichment process, process step is following:
A, vacuum tightness-0.08～-0.09Mpa under, it is 105～110 ℃ that heating concentrates distillation residual liquid to temperature of charge, and sodium-chlor is separated out from raffinate;
B, close vacuum, emptying continues to be heated to temperature of charge and reaches 130～135 ℃, makes the sodium formiate dissolving that crystallization is separated out in the raffinate vacuum Concentrating Process;
After C, temperature of charge reach 130～135 ℃, material is put into the strainer with the jacketed of steam heating insulation, vacuum filtration makes the sodium-chlor of separating out in the material separate with material solution;
D, the material solution of suction filtration gained is put into crystallization kettle, add the methyl alcohol of about 1/4 material solution volume, after conventional extraction, crystallization,, obtain the low recovery sodium formiate of sodium chloride as impurity content again through press filtration, drying process.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710301A (en) * | 2014-04-29 | 2015-06-17 | 杨胜利 | Process for recovering sodium formate from sodium hydrosulfite raffinate |
| CN106706841A (en) * | 2016-12-13 | 2017-05-24 | 柳州化工股份有限公司 | Method for analyzing purity of recycled sodium formate during sodium hydrosulfite production |
| CN107032981A (en) * | 2017-05-02 | 2017-08-11 | 山东博苑医药化学有限公司 | A kind of method recycled containing sodium formate and sodium chloride mixing solid wastes recycling |
| CN114057610A (en) * | 2021-11-30 | 2022-02-18 | 湖北省宏源药业科技股份有限公司 | Production method of high-purity guanidine thiocyanate |
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| CN1459444A (en) * | 2003-05-29 | 2003-12-03 | 烟台市金河保险粉厂有限公司 | Method of producing sodium formate using crude methyl alcohol rectification residual liquid in production of sodium hydrosulfite |
| CN102050471A (en) * | 2010-11-05 | 2011-05-11 | 烟台大学 | Method for recycling sodium formate and sodium sulfite from waste sodium hydrosulfite liquid with sodium formate method |
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2012
- 2012-07-13 CN CN2012102429915A patent/CN102746134A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1459444A (en) * | 2003-05-29 | 2003-12-03 | 烟台市金河保险粉厂有限公司 | Method of producing sodium formate using crude methyl alcohol rectification residual liquid in production of sodium hydrosulfite |
| CN102050471A (en) * | 2010-11-05 | 2011-05-11 | 烟台大学 | Method for recycling sodium formate and sodium sulfite from waste sodium hydrosulfite liquid with sodium formate method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104710301A (en) * | 2014-04-29 | 2015-06-17 | 杨胜利 | Process for recovering sodium formate from sodium hydrosulfite raffinate |
| CN106706841A (en) * | 2016-12-13 | 2017-05-24 | 柳州化工股份有限公司 | Method for analyzing purity of recycled sodium formate during sodium hydrosulfite production |
| CN107032981A (en) * | 2017-05-02 | 2017-08-11 | 山东博苑医药化学有限公司 | A kind of method recycled containing sodium formate and sodium chloride mixing solid wastes recycling |
| CN107032981B (en) * | 2017-05-02 | 2018-07-03 | 山东博苑医药化学有限公司 | A kind of method recycled containing sodium formate and sodium chloride mixing solid wastes recycling |
| CN114057610A (en) * | 2021-11-30 | 2022-02-18 | 湖北省宏源药业科技股份有限公司 | Production method of high-purity guanidine thiocyanate |
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Application publication date: 20121024 |