CN101597250A - Acid copper intermediate sodium polydithio-dipropyl sulfonate synthetic method - Google Patents
Acid copper intermediate sodium polydithio-dipropyl sulfonate synthetic method Download PDFInfo
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- CN101597250A CN101597250A CNA200810047928XA CN200810047928A CN101597250A CN 101597250 A CN101597250 A CN 101597250A CN A200810047928X A CNA200810047928X A CN A200810047928XA CN 200810047928 A CN200810047928 A CN 200810047928A CN 101597250 A CN101597250 A CN 101597250A
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- copper intermediate
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 14
- 239000010949 copper Substances 0.000 title claims abstract description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 title claims abstract description 12
- -1 polydithio-dipropyl Polymers 0.000 title claims abstract description 12
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 12
- 239000011734 sodium Substances 0.000 title claims abstract description 12
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 title claims abstract description 12
- 238000010189 synthetic method Methods 0.000 title claims abstract description 9
- 239000002253 acid Substances 0.000 title description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 10
- 230000008025 crystallization Effects 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 8
- 238000004064 recycling Methods 0.000 claims abstract description 6
- 230000003647 oxidation Effects 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract 2
- 238000004821 distillation Methods 0.000 claims abstract 2
- 238000001035 drying Methods 0.000 claims abstract 2
- 238000006386 neutralization reaction Methods 0.000 claims abstract 2
- 238000001953 recrystallisation Methods 0.000 claims abstract 2
- 239000002904 solvent Substances 0.000 claims abstract 2
- 238000003786 synthesis reaction Methods 0.000 claims abstract 2
- 239000000047 product Substances 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000012043 crude product Substances 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 238000007747 plating Methods 0.000 description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 4
- 238000005282 brightening Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000002860 competitive effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- SRRKNRDXURUMPP-UHFFFAOYSA-N sodium disulfide Chemical compound [Na+].[Na+].[S-][S-] SRRKNRDXURUMPP-UHFFFAOYSA-N 0.000 description 2
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 description 1
- ZTWXTOUATKTCQF-UHFFFAOYSA-N 3-hydroxypropane-1-sulfonic acid;sodium Chemical compound [Na].OCCCS(O)(=O)=O ZTWXTOUATKTCQF-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of sour copper intermediate sodium polydithio-dipropyl sulfonate (SPS) synthetic method, comprise reactions steps such as neutralization reaction and oxidizing reaction, obtain finished product through concentrated, crystallization, drying, recrystallization again.Be primarily characterized in that the sour copper intermediate SPS that obtains content 90% after the intermediate oxidation of synthesis of high content, the alcohol solvent distillation back recycling in the reaction process.This method can effectively reduce environmental pollution, reduce labour intensity, and product cost is low, and the market competitiveness is strong.
Description
Technical field:
The present invention relates to a kind of sour copper intermediate sodium polydithio-dipropyl sulfonate (SPS) synthetic method.
Background technology:
SPS chemistry sodium polydithio-dipropyl sulfonate by name is mainly used in the plating acid copper-plating.As the acid copper-plating intermediate, belong to the main interpolation composition in the copper plating additive, can play coating crystallization refinement, the effect that effectively improves current density of making.On whole sour copper brightening agent market, this product consumption is very big, and effect is good.On the market, sour copper brightening agent product is not only monopolizing domestic most of market, and is costing an arm and a leg mainly with the form import of finished product at home.Home-made acid copper brightening agent, client's ordinary priority selects for use import SPS to add, and its content can reach 80-90%, and impurity is few, but because product price is higher, brings certain competitive pressure to the client.And more domestic producers, because technology etc. are all multifactor, the content of producing SPS is at 50-60%, and purity is not enough, and impurity is many, has limited the application in market at home.In order to change SPS sale predicament at home, seek a kind of synthetic method that improves SPS content and purity, have great importance.
Summary of the invention:
Obtain consulting a large amount of documents and materials, the method for synthetic SPS mainly contains following three kinds of methods at present:
(1) thiocarbamide method: promptly synthetic with thiocarbamide and 3-hydroxypropanesulfonic acid sodium.But this method step is very loaded down with trivial details, produces four steps of the minimum needs of product from being dosed into, and the yield in each step is not high, and the productive rate that draws at last is very low, has only about 40%, and content also has only about 80%, unsuitable suitability for industrialized production.
(2) sodium disulfide method: promptly with Na2S2 and the reaction of propane sultone.Subject matter is, analyzes content with this method synthetic product with chemical analysis and can reach 90%, but have only 50-60% with the liquid chromatograph analysis, and foreign matter content wherein is very high.。
(3) oxidation style: sodium polydithio-dipropyl sulfonate is synthesized in oxidation, and products obtained therefrom SPS detects gained content by HPLC can reach 80-90%.
According to a large amount of research relatively, determined to synthesize the technology of sodium polydithio-dipropyl sulfonate with oxidation style.In order to select best processing condition, carried out the reaction under the various conditions, as changing proportioning raw materials, the temperature of reaction of reaction, oxygenant etc.The product yield that draws in this way is higher.Update and adjust production technique through I technician of company, successfully synthesize the sodium polydithio-dipropyl sulfonate of content 85-90%.
Concrete reactions steps is as follows:
1. the product after will neutralizing is dissolved in the pure water, adds oxygenant oxidation reaction, and temperature 5-15 degree reacted 3 hours.
2. the reaction times heats up to the back and has been concentrated into crystallization and separates out, and adds an amount of ethanol, separates out mass crystallization, cooling.
3. temperature is reduced to 5 and is filtered when spending, and obtains the SPS crude product of content 80-85% after the filter cake oven dry.
4. the SPS crude product is joined in an amount of 85% ethanolic soln, add the decolorizing with activated carbon removal of impurities after the rising temperature for dissolving, remove by filter carbon dust.
5. filtrate cooling is separated out, and 5 filter when spending, and filtration cakes torrefaction promptly gets high-content SPS product.Filtrate recycling ethanol.
Significance dominance of the present invention is: technological operation is simple, and side reaction is few, and the product aftertreatment is simple, and is with short production cycle, for energy-saving and emission-reduction contribute.And price has competitive power only for 1/2nd of import like product on market.
Embodiment:
Below in conjunction with preferred embodiment, details are as follows to embodiment provided by the invention:
Embodiment 1:
Reactions steps:
(1) is dissolved in the pure water with after product among the general, adds oxygenant A, oxidization time 24 hours, oxidizing temperature 80-100 degree.
(2) reaction times arrives, and adds 5 ‰ gacs in solution, and 60-80 degree decolouring removal of impurities 1 hour removes by filter gac.
(3) filtrate has been concentrated to crystal when separating out, and adds an amount of ethanol, separates out mass crystallization, cooling.
(4) temperature is reduced to 5 and is filtered when spending, and obtains the SPS crude product of content 80-85% after the filter cake oven dry.
(5) the SPS crude product is joined in an amount of 85% ethanolic soln, add the decolorizing with activated carbon removal of impurities after the rising temperature for dissolving, remove by filter carbon dust.
(6) filtrate cooling is separated out, and 5 filter when spending, and filtration cakes torrefaction promptly gets content 85-90%SPS product.Filtrate recycling ethanol.
Embodiment 2:
Reactions steps:
(1) product after will neutralizing is dissolved in the pure water, adds oxygenant B oxidizing reaction, and temperature 5--15 degree reacted 3 hours.
(2) reaction times heats up to the back and has been concentrated into crystallization and separates out, and adds an amount of ethanol, separates out mass crystallization, cooling.
(3) temperature is reduced to 5 and is filtered when spending, and obtains the SPS crude product of content 80-85% after the filter cake oven dry.
(4) the SPS crude product is joined in an amount of 85% ethanolic soln, add the decolorizing with activated carbon removal of impurities after the rising temperature for dissolving, remove by filter carbon dust.
(5) filtrate cooling is separated out, and 5 filter when spending, and filtration cakes torrefaction promptly gets content 85-90%SPS product.Filtrate recycling ethanol.
Claims (4)
1. a sour copper intermediate sodium polydithio-dipropyl sulfonate (SPS) synthetic method comprises reactions steps such as neutralization reaction and oxidizing reaction, obtains finished product through concentrated, crystallization, drying, recrystallization again.Be primarily characterized in that the sour copper intermediate SPS that obtains content 90% after the intermediate oxidation of synthesis of high content, the alcohol solvent distillation back recycling in the reaction process.Its feature process is as follows:
(1) product after will neutralizing is dissolved in the pure water, adds oxygenant oxidation reaction.
(2) reaction times heats up to the back and has been concentrated into crystallization and separates out, and adds an amount of ethanol, separates out mass crystallization, cooling.
(3) cooling after-filtration obtains the SPS crude product of content 80-85% after the filter cake oven dry.
(4) the SPS crude product is joined in an amount of certain density ethanolic soln, add the decolorizing with activated carbon removal of impurities after the rising temperature for dissolving, remove by filter carbon dust.
(5) the filtrate cooling is separated out, and filters, and filtration cakes torrefaction promptly gets content 85-90%SPS product.Filtrate recycling ethanol.
2. sour copper intermediate sodium polydithio-dipropyl sulfonate according to claim 1 (SPS) synthetic method is characterized in that: the oxidizer temperature of reaction is the 5-15 degree in the described step (1).
3. sour copper intermediate sodium polydithio-dipropyl sulfonate according to claim 1 (SPS) synthetic method is characterized in that: the cooling temperature is 5 degree before filtering in the described step (3).
4. sour copper intermediate sodium polydithio-dipropyl sulfonate according to claim 1 (SPS) synthetic method is characterized in that: ethanolic soln concentration is 85% in the described step (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810047928XA CN101597250A (en) | 2008-06-05 | 2008-06-05 | Acid copper intermediate sodium polydithio-dipropyl sulfonate synthetic method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA200810047928XA CN101597250A (en) | 2008-06-05 | 2008-06-05 | Acid copper intermediate sodium polydithio-dipropyl sulfonate synthetic method |
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| CN101597250A true CN101597250A (en) | 2009-12-09 |
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| CNA200810047928XA Pending CN101597250A (en) | 2008-06-05 | 2008-06-05 | Acid copper intermediate sodium polydithio-dipropyl sulfonate synthetic method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606738A (en) * | 2016-02-05 | 2016-05-25 | 湖北吉和昌化工科技有限公司 | HPLC (High Performance Liquid Chromatography) analysis method for sodium 3,3'-dithiodipropane sulfonate |
| CN108914171A (en) * | 2018-07-19 | 2018-11-30 | 广东工业大学 | A kind of acceleration copper deposition additive and its preparation method and application |
| CN114232041A (en) * | 2022-01-17 | 2022-03-25 | 中国计量大学 | A kind of high aspect ratio blind hole copper filling electroplating solution and preparation method thereof |
| CN114853645A (en) * | 2022-04-22 | 2022-08-05 | 苏州亚科科技股份有限公司 | A kind of preparation technology of sodium polydisulfide dipropane sulfonate |
| CN115611791A (en) * | 2022-11-03 | 2023-01-17 | 湖北吉和昌化工科技有限公司 | Preparation method of sodium polydithio-dipropyl sulfonate |
-
2008
- 2008-06-05 CN CNA200810047928XA patent/CN101597250A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105606738A (en) * | 2016-02-05 | 2016-05-25 | 湖北吉和昌化工科技有限公司 | HPLC (High Performance Liquid Chromatography) analysis method for sodium 3,3'-dithiodipropane sulfonate |
| CN108914171A (en) * | 2018-07-19 | 2018-11-30 | 广东工业大学 | A kind of acceleration copper deposition additive and its preparation method and application |
| CN114232041A (en) * | 2022-01-17 | 2022-03-25 | 中国计量大学 | A kind of high aspect ratio blind hole copper filling electroplating solution and preparation method thereof |
| CN114232041B (en) * | 2022-01-17 | 2023-11-21 | 中国计量大学 | High-depth-diameter-ratio blind hole copper filling electroplating solution and preparation method thereof |
| CN114853645A (en) * | 2022-04-22 | 2022-08-05 | 苏州亚科科技股份有限公司 | A kind of preparation technology of sodium polydisulfide dipropane sulfonate |
| CN115611791A (en) * | 2022-11-03 | 2023-01-17 | 湖北吉和昌化工科技有限公司 | Preparation method of sodium polydithio-dipropyl sulfonate |
| CN115611791B (en) * | 2022-11-03 | 2023-12-26 | 湖北吉和昌化工科技有限公司 | Preparation method of sodium polydithio-dipropyl sulfonate |
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Application publication date: 20091209 |