CN1025562C - Preparation process of hydroxyalkanesulfonic acid for electroplating solution - Google Patents
Preparation process of hydroxyalkanesulfonic acid for electroplating solution Download PDFInfo
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- CN1025562C CN1025562C CN 89103987 CN89103987A CN1025562C CN 1025562 C CN1025562 C CN 1025562C CN 89103987 CN89103987 CN 89103987 CN 89103987 A CN89103987 A CN 89103987A CN 1025562 C CN1025562 C CN 1025562C
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- CN
- China
- Prior art keywords
- acid
- hydroxyl alkyl
- metal salt
- alkali metal
- preparation process
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
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- 239000002253 acid Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000009713 electroplating Methods 0.000 title abstract description 14
- -1 alkali metal salt Chemical class 0.000 claims abstract description 29
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920005989 resin Polymers 0.000 claims description 9
- 230000007704 transition Effects 0.000 claims description 8
- 238000005342 ion exchange Methods 0.000 claims description 5
- 239000003729 cation exchange resin Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 159000000000 sodium salts Chemical group 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 238000007747 plating Methods 0.000 abstract description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 abstract 1
- 230000000694 effects Effects 0.000 abstract 1
- LQBJWKCYZGMFEV-UHFFFAOYSA-N lead tin Chemical compound [Sn].[Pb] LQBJWKCYZGMFEV-UHFFFAOYSA-N 0.000 abstract 1
- 231100000956 nontoxicity Toxicity 0.000 abstract 1
- 239000002699 waste material Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 14
- 239000000243 solution Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 7
- 239000003456 ion exchange resin Substances 0.000 description 6
- 229920003303 ion-exchange polymer Polymers 0.000 description 6
- 239000003513 alkali Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000010828 elution Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 235000015424 sodium Nutrition 0.000 description 3
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 2
- CLHYKAZPWIRRRD-UHFFFAOYSA-N 1-hydroxypropane-1-sulfonic acid Chemical compound CCC(O)S(O)(=O)=O CLHYKAZPWIRRRD-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 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 description 2
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910000648 terne Inorganic materials 0.000 description 2
- HSXUNHYXJWDLDK-UHFFFAOYSA-N 2-hydroxypropane-1-sulfonic acid Chemical compound CC(O)CS(O)(=O)=O HSXUNHYXJWDLDK-UHFFFAOYSA-N 0.000 description 1
- WQPMYSHJKXVTME-UHFFFAOYSA-N 3-hydroxypropane-1-sulfonic acid Chemical compound OCCCS(O)(=O)=O WQPMYSHJKXVTME-UHFFFAOYSA-N 0.000 description 1
- 229910000978 Pb alloy Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- NQKHODGWABEJEI-UHFFFAOYSA-N [SiH3]S(=O)(=O)OO Chemical compound [SiH3]S(=O)(=O)OO NQKHODGWABEJEI-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 229940023913 cation exchange resins Drugs 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-N sulfonic acid Chemical compound OS(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-N 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A preparation process of hydroxyalkanesulfonic acid for electroplating process, and the product is widely used for electroplating process. Using alkali metal salt of hydroxy alkane sulfonic acid as raw material, using solid Ba (OH)2·8H2O will be harmful SO therein4 -SO3 -The method has the advantages of simple operation, good effect, greatly reduced production cost, no toxicity, simplified three-waste treatment, energy consumption saving and the like, and the prepared product is particularly suitable for tin-lead electroplating process, can obtain excellent plating layer and has full-bright appearance.
Description
The present invention is a kind of preparation method who is used for the industrial chemicals of electroplate liquid, and its product is mainly used in electroplating technologies such as tinsel.
Terne Electroplating technology mainly adopts fluoroborate production both at home and abroad at present, the employing thionamic acid that also has-tin fluoborate lead alloy electroplating technology, citric acid Terne Electroplating technology, but all have its limitation in the use.Though existing people finds to adopt hydroxyl alkyl sulphonic acid as the electroplate liquid main raw material, weigh result of use comprehensively and also confirmed to be better than above-mentioned various electroplate liquid raw material, just hydroxyl alkyl sulphonic acid does not still have and finds the approach of producing economically and reasonably, and production cost is higher, so promotion rate is restricted.According to Japanese publication communique; the record of clear 57-171958 patent; adopt the intermediate product of mineral acid or ion exchange resin treatment r-halopropyl acylate and alkali sulfite reacting metal salt gained, thereby produce cyclic lactone (1-hydroxy-propanesulfonic acid lactone) by the intramolecularly esterification.As seen this patent can only be the product that r-halopropyl acylate and alkali sulfite reacting metal salt obtain with mineral acid or the ion exchange resin object of handling that makes the transition; be an alkali metal salt of 1-hydroxy-propanesulfonic acid-3, and its final product is the ring lactones of 1-hydroxy-propanesulfonic acid.This method is before adopting ion exchange resin processing transition, middle product is not carried out this technological process of removal of impurities, and treatment process also has the specific requirement of itself, and anionic impurity can't be removed in the 1-hydroxy-propanesulfonic acid after the processing, particularly contains a large amount of cl
-, therefore on electroplating technology, can't use fully, the hydroxyl alkyl sulphonic acid that obtain being used for electroplating technology must find a new way.
Purpose of the present invention just is to provide a kind of preparation method who is used for the hydroxyl alkane sulphur liquid of electroplate liquid, is fit to the requirement of industrialization electroplating technology, makes every effort to economical, effective.
The raw material of this technology is an alkali metal salt of hydroxyl alkyl sulphonic acid, can be: an alkali metal salt of 2-ethylenehydrinsulfonic acid or 2-hydroxy-propanesulfonic acid or 3-hydroxy-propanesulfonic acid or 2-hydroxyl fourth sulfonic acid.Earlier through removing to the deleterious SO of electroplating technology
= 4, SO
= 3Deng impurity, handle transition through ion exchange resin again, produce the corresponding hydroxyl alkyl sulphonic acid that is applicable to electroplating technology.The also available similar approach of other lower alkanes sulfonate sodiums makes the transition.The described an alkali metal salt of this technology is preferably sodium salt, and described ion exchange resin is storng-acid cation exchange resin, and as 732,733,734,742JK006 etc., the hydroxyl alkyl sulphonic acid an alkali metal salt that this technology is suitable for is usually by following method preparation and get:
Wherein R represents H or CH
3, C
2H
5
Specific operation process is as follows:
The weight percent that in the hydroxyl alkyl sulphonic acid alkali metal salt soln, adds 3～10%(pure substance) solid-state Ba(OH
2)
28H
2O stirred under the room temperature 0.5～1 hour, left standstill after mixing 12～48 hours, got upper strata settled solution BaCl
2Check SO
= 4, SO
3Whether Ex-all if muddy the generation arranged, then need be added Ba(OH as one feels fit)
28H
2O is until confirming no SO
= 4, SO
= 3Till the existence, to leave standstill liquid then and remove by filter throw out, clarifying filtered liquid makes the transition for ion-exchange, with being highly acid Zeo-karb through regeneration, the an alkali metal salt of hydroxyl alkyl sulphonic acid is made the transition acid, at room temperature, treatment solution flows through the storng-acid cation exchange resin bed with certain take-off rate, flow out liquor capacity and the concentration value of moment by measuring it, can draw elution curve, for example: adopting 732 storng-acid cation exchange resins, the resin volume is 60 liters, and the treatment solution flow is 15 liters/hour, concentration is under the 2.2N condition, can draw its elution curve such as accompanying drawing:
Wherein starting point 0 be in exit acidity to pH=4 hour, the beginning cumulative throughflow is measured concentration.
According to elution curve, the unit volume exchange resin can be calculated and the quantitative range of certain density hydroxy silane sulfonate can be handled, from curve, also can judge leakage point simultaneously, calculate the width of exchange zone, thereby reasonably design switch and control whole exchange process effectively.
When cation exchange reaction, the control of the take-off rate of treatment solution is most important, and the take-off rate of this technology is generally 0.1～0.4 liter/hour and rises resin.Handled the ion exchange resin bed of solution, available 5～10% hydrochloric acid (technical pure) regeneration imports with the reverse direction with the above-mentioned treatment solution flow direction, and its flow velocity is generally 0.1～0.4 liter/hour and rises resin.Its usage quantity is about 2～3 times of exchange resin volume, then with the washed with de-ionized water of 3～9 times of resin volumes, and must be cl
-Ion all cleans up.Regenerative operation at room temperature carries out, and ion exchange bed just can reuse after above-mentioned manipulation of regeneration.
Product after ion exchange reaction has dilution to a certain degree, can adopt vacuum-evaporation to concentrate for ease of transportation.The final concentration usable acid alkali titration quantitative analysis of product is determined.
Below provide embodiments of the invention and technological process further specified:
Get 60 liters of commercially available 2-ethylenehydrinsulfonic acid sodium stostes, content is generally 32%, adds CP level Ba(OH)
28H
2O, 1800 grams stirred 40 minutes, milky white precipitate occurred, leave standstill 24 hours after, top clear liquor dropping 0.5%BaCl takes a morsel
2Solution check SO
= 4, SO
= 3Whether react completely,, add the Ba(OH about 1～2 grams per liter again) if muddiness is arranged
28H
2O until reacting completely, removes by filter throw out then, obtains pure 2-ethylenehydrinsulfonic acid sodium solution.The two positive post series connection fixed-bed resin volume that adopts 732 highly acidic cations exchange ester to form is 60 liters, treatment solution after purifying is carried out ion-exchange transition with 0.25 liter of/hour take-off rate that rises resin from top to bottom, obtain the 2-ethylenehydrinsulfonic acid that 70～90 liters of concentration are about 1.8N at last, its turnover ratio is more than 95%.
This technological operation is simple, and production cost reduces greatly, has steady quality, and product is nontoxic, saves advantages such as energy consumption.The product that makes is specially adapted to the plumbous electroplating technology of tin, and coating performance is good, and the coating appearance reaches complete bright level, satisfies the requirement of Ministry of Electronics Industry's standard laid down by the ministries or commissions of the Central Government regulation fully, has wide promotion prospect.
Claims (2)
1, a kind of preparation process of hydroxyl alkyl sulfonic acid that is used for electroplate liquid, it is characterized in that adopting an alkali metal salt of hydroxyl alkyl sulphonic acid is raw material, make the transition through removal of impurities and ion-exchange, specific embodiment is: the solid Ba (OH that adds 3～10% (weight percents of pure substance) in the alkali metal salt soln of hydroxyl alkyl sulphonic acid
2) 8H
2O stirred after 0.5～1 hour, left standstill 12～48 hours, remove by filter throw out then, at room temperature, clarifying filtrate is flow through the storng-acid cation exchange resin bed with 0.1～0.4 liter of/hour take-off rate that rises resin, said hydroxyl alkyl sulphonic acid an alkali metal salt, produce by following approach:
Wherein R represents H or CH
3Or C
2H
5
2, a kind of preparation process of hydroxyl alkyl sulfonic acid that is used for electroplate liquid as claimed in claim 1 is characterized in that said hydroxyl alkyl sulphonic acid an alkali metal salt is a sodium salt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89103987 CN1025562C (en) | 1989-06-14 | 1989-06-14 | Preparation process of hydroxyalkanesulfonic acid for electroplating solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 89103987 CN1025562C (en) | 1989-06-14 | 1989-06-14 | Preparation process of hydroxyalkanesulfonic acid for electroplating solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1038806A CN1038806A (en) | 1990-01-17 |
| CN1025562C true CN1025562C (en) | 1994-08-03 |
Family
ID=4855378
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 89103987 Expired - Fee Related CN1025562C (en) | 1989-06-14 | 1989-06-14 | Preparation process of hydroxyalkanesulfonic acid for electroplating solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1025562C (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102389630B1 (en) | 2016-06-30 | 2022-04-21 | 피피지 인더스트리즈 오하이오 인코포레이티드 | Electrodepositable coating composition having improved crater control |
-
1989
- 1989-06-14 CN CN 89103987 patent/CN1025562C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1038806A (en) | 1990-01-17 |
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