CN108912022A - A kind of method of purification of sodium polydithio-dipropyl sulfonate - Google Patents
A kind of method of purification of sodium polydithio-dipropyl sulfonate Download PDFInfo
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- CN108912022A CN108912022A CN201810835209.8A CN201810835209A CN108912022A CN 108912022 A CN108912022 A CN 108912022A CN 201810835209 A CN201810835209 A CN 201810835209A CN 108912022 A CN108912022 A CN 108912022A
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- Prior art keywords
- sodium
- exchange resin
- dipropyl sulfonate
- purification
- resin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
Abstract
The invention belongs to chemicals purification technique fields, and in particular to a kind of new method of purification of sodium polydithio-dipropyl sulfonate；The sodium polydithio-dipropyl sulfonate mother liquor that our company's patent CN106946753A method synthesizes first is passed sequentially through alkalescence anion-exchange resin, passes through acid cation exchange resin by the present invention, the sodium sulfate salt in removing system；Then regulation system pH value is to 3-7, successively by concentration, cooling, centrifugation, drying；The sodium polydithio-dipropyl sulfonate for finally obtaining high-purity, not only purity and content are high but also economic and environment-friendly for the sodium polydithio-dipropyl sulfonate obtained through present invention purification, are easily industrialized.
Description
Technical field
The invention belongs to chemicals purification technique fields, and in particular to a kind of purification of new sodium polydithio-dipropyl sulfonate
Method.
Background technique
Sodium polydithio-dipropyl sulfonate (Bis- (3-sullfopropyl) disulfide, hereinafter referred to as SPS), molecular formula：
C6H12Na2O6S4, molecular weight：354.40 No. CAS：27206-35-5, white are mainly used for acid plating to faint yellow solid powder
Coating decorative and functional can be obtained (such as in copper brightener：Printed circuit board).SPS can be formulated with typical copper facing in as non-
Ionic surface active agent, polyamine and other sulfhydryl compounds are used in combination, and can also be used in combination with dyestuff, if in conjunction with N,
N- dimethyl-dithio carbonyl propane sulfonic acid sodium (DPS) and 3- (benzothiazole -2- sulfydryl)-propane sulfonic acid sodium (ZPS) or thiocarbamide
Propyl sulfate (UPS) uses, it will obtains more preferably effect.As acid copper-plating intermediate, belong to the master in copper plating additive
Composition is added, can play the role of making coating crystallization refinement, effectively improve current density.In the market of entire brightening agent for acid copper electroplating
On, this product consumption is very big, and application effect is excellent.
In order to reach optimum efficiency, it is necessary to use the higher sodium polydithio-dipropyl sulfonate of purity.In the prior art, main
The sodium chloride salt (such as Chinese patent CN106748934A) in nanofiltration membrane removing system is used, but its purity is much not achieved
The requirement of market economy and people to high-quality.
Summary of the invention
To solve the above-mentioned problems, the purpose of the present invention is to provide a kind of purifications of new sodium polydithio-dipropyl sulfonate
Method；This method is not only simple and easy, of less demanding to production equipment, but also the final products content that purification obtains is high, purity
Height, it is economic and environment-friendly, be easily industrialized.
The present invention is achieved through the following technical solutions：
A kind of method of purification of sodium polydithio-dipropyl sulfonate, specially：First by the poly- two sulphur dipropyl containing sodium sulfate salt
Alkyl sulfonic acid mother liquid of sodium passes sequentially through alkalescence anion-exchange resin, passes through acid cation exchange resin；Then regulation system pH
Value successively passes through concentration, cooling, is centrifuged, is dry to 3-7；Finally obtain high-purity sodium polydithio-dipropyl sulfonate.
Preferably, the content of sodium sulfate salt is 3-5%, polydithio-dipropyl in the sodium polydithio-dipropyl sulfonate mother liquor
The content of sodium sulfonate is 20-30%.
Preferably, the sodium polydithio-dipropyl sulfonate mother liquor containing sodium sulfate salt is our company's patent
CN106946753A implements mother liquor obtained.I.e. first using 1,3-propane sultone as raw material, with sulphur sodium thiosulfuric acid in alcohols material
Preparation Peng Te salt is reacted with the in the mixed solvent of water, and then Peng Te salt obtained is alkalized and aoxidized again, is obtained containing SPS's
Mother liquor, sodium sulfate salt content is 3-5% in mother liquor, and SPS content is 20-30%.
Preferably, it is macropore alkalinity acrylic acid that the alkalescence anion-exchange resin, which is the alkalescence anion-exchange resin,
Series anion exchange resin, macropore basicity styrene series anion exchange resin or macropore polystyrene chelating ion exchange resin
One or more of composition.
Preferably, the alkalescence anion-exchange resin be containing：
-N+(CH3)3The alkalescence anion-exchange resin of the comprehensive functional group of one or more of OH functional group.
Wherein, macropore alkalinity acrylic acid type anion exchange resin is optional：D318, D317, D213, D311, KP-7055 etc.
Oleic series anion exchange resin；The benzene such as macropore basicity styrene series anion exchange resin optional D301, D201, D301
Ethylene series anionic exchanger resin；Macropore polystyrene chelating ion exchange resin optional D401, D402 etc..
KP-7055 model resin is that flat resin is opened using special synthetic technology synthesis with multi-functional production in Shanghai
Product, exchange capacity is high, and regeneration efficiency is high；The acid ion being mainly used in separation organic matter；D301 type resin is macropore
The weak-base anion-exchange resin that tertiary amine groups are had in the styrene-divinylbenzene copolymer of structure, can effectively remove body
Inorganic acid and silicate in system；D318 type resin is the methyl acrylate copoly cross-linked polymer polymer of macroporous structure, is led to
It crosses polyethylene polyamine and carries out the polyamines base weak-base anion-exchange resin that aminolysis obtains, exchange capacity is big, high mechanical strength
Feature.Mainly using the sulfate radical in KP-7055 and D301 model anion exchange resin removing system in this product, to reach
Improve the purpose of content.
Preferably, the dosage of the alkalescence anion-exchange resin is：Sulfate radical content and alkalescence anion-exchange resin
Capacity ratio be 1:1-10.
Preferably, the acid cation exchange resin is macroreticular acidic acrylic acid type cation exchange resin, macropore acid
One or both of property styrene type cation exchange resin composition.
Preferably, the acid cation exchange resin be containing：
The acid cation exchange resin of functional group.
Optional D113 of macroreticular acidic acrylic acid type cation exchange resin etc., macroreticular acidic polystyrene cation exchange tree
The styrene type cation exchange resins such as rouge optional D001,001*7, WD011.
001*7 is to synthesize on the basis of based on 001 resin by specific process with WD001, and 001 resin of comparison is more
Greatly, and structure is more stable, is fallen off under strongly alkaline conditions using not having small molecule.D113 is macropore acidulous acrylic acid system
Cation exchange resin, exchange capacity is high, and volume change is small.
Preferably, the acid cation exchange resin dosage of stating is：Sodium polydithio-dipropyl sulfonate states acidity with described
The exchange capacity ratio of cation exchange resin is 1:1-10.
The principle of the present invention is will to contain 20-30%SPS, and 3-5% sulfuric acid mother liquid of sodium passes through basic anionic resin, selection
Sexual intercourse swaps out sulfate radical in mother liquor, reaches desalination purpose, improves product content；Again by the mother liquor after desalination by faintly acid sun from
Subtree rouge, regulation system pH to faintly acid, is precipitated impurity, and removal of impurities purpose is reached after adding carbon dust to adsorb, and improves product purity.This
Resin anion (R.A.) is activated using 3-10%NaOH solution in invention, and resin cation is activated using 2-10% dilution heat of sulfuric acid, yin
Solution after resin cation activation mutually neutralizes, and sodium sulfate byproduct salt is packed after collecting and sold.
Sulfate of the anion exchange resin effectively in removing system has been respectively adopted in the present invention, improves product content；
The impurity in SPS is effectively removed using cation exchange resin, improves the purity of product, products obtained therefrom high income, content be high,
Purity is high, economy, are easily industrialized environmental protection.
Specific embodiment
The present invention is described in further detail With reference to embodiment, to help those skilled in the art's reason
The solution present invention.
Embodiment 1
1) SPS mother liquor 1000ml is taken, SPS 28.3%, sodium sulphate 4.78% are contained, it is 97.32% that liquid phase, which detects its purity,
It is warming up to 45-60 DEG C；
It 2) is 2- by the time by above-mentioned mother liquor by hydrogen-oxygen type resin anion (R.A.) KP-7055, amount of resin 147ml
3h；
Taking and detecting its SPS content by resin anion (R.A.) post mother liquor is 27.15%, sodium sulphate 0.08%, liquid phase detection
Its purity is 98.35%, system pH most 12.95；
It 3) is 2-4h by the time by above-mentioned mother liquor by hydrogen form cation resin WD001, amount of resin 78ml；
Taking and detecting its SPS content by resin cation post mother liquor is 27.15%, sodium sulphate 0.08%, liquid phase detection
Its purity is 99.85%, system pH most 5.2；
4) by the complete mother liquor of above-mentioned processing using being dehydrated after activated carbon adsorption to doing, then dry drying, obtains solid：
271g, detecting its solid content is 99.3%, sodium sulphate content 0.29%, purity 99.91%, and water-soluble qualified, pH is
5.65.Product yield is:95.75%.
Embodiment 2
1) SPS mother liquor 1000ml is taken, detecting its SPS content is 28.9%, sulfate radical content 4.93%, and purity is
96.32%；
2) D301 resin 200ml is added into resin absorbing column, mother liquor SPS is added thereto, it is made to slow transit through absorption
Column, time between 1-4h, maintain the temperature at 30-50 DEG C；
It will be detected by D301 resin post mother liquor, SPS content is 26.5%, sodium sulphate content 1.32%, and purity is
97.01%；
3) above-mentioned mother liquor is added into the resin absorbing column equipped with D113 resin 200ml, it is made to slow transit through adsorption column, when
Between between 2-4h, maintain the temperature at 30-50 DEG C；
It will be detected by D113 resin post mother liquor, SPS content is 26.3%, sulfate radical 1.24%, and purity is
99.31%；
4) mother liquor is using 1.35g active carbon in 30-60 DEG C of absorption 2-4h, filtering means dehydration to dry, drying.Obtain solid
253g, detecting its content is 94.33%, sodium sulphate content 5.2%, purity 99.65%, product yield 87.54%.
Embodiment 3
1) SPS mother liquor 1000ml is taken, detecting its SPS content is 28.9%, sulfate radical content 4.93%, and purity is
96.32%；
2) KP-7055 resin 150ml is added into resin absorbing column, mother liquor SPS is added thereto, it is made to slow transit through suction
Attached column, time between 2-4h, maintain the temperature at 30-40 DEG C；
It will be detected by KP-7055 resin post mother liquor, SPS content is 27.68%, sodium sulphate content 0.06%, purity
It is 97.53%；
3) above-mentioned mother liquor is added into the resin absorbing column equipped with WD001 resin 80ml, it is made to slow transit through adsorption column, when
Between between 2-4h, maintain the temperature at 40-60 DEG C；
It will be detected by WD001 resin post mother liquor, SPS content is 27.58%, sulfate radical 0.06%, and purity is
99.89%；
4) mother liquor is using 1.5g active carbon in 30-60 DEG C of absorption 2-4h, filtering means dehydration to dry, drying.Solid 272g is obtained,
Detecting its content is 99.54%, sodium sulphate content 0.22%, purity 99.73%, product yield 94.12%.
Above-described embodiment, only presently preferred embodiments of the present invention, is not intended to limit the invention practical range, therefore all with this
The equivalent change or modification that feature described in invention claim and principle are done should all be included in scope of the invention as claimed
Within.
In conclusion the method that the present invention purifies SPS is effective.By experimental demonstration repeatedly, from absorption temperature
Degree, amount of resin, adsorption rate etc. have done a large amount of lab scales, and using different hydrogen-oxygen type anion exchange resin to sulphur in reaction solution
Acid group absorption comparison, different hydrogen type cation exchange resins purify reaction solution and compare, and the product content made reaches
99.54%, purity reaches 99.89%, and yield is 94% or more, and the stable product quality, exterior beauty is good, and electroplating effect is excellent
It is good.Company standard is met using the SPS that present invention process technology purifies, effectively raises the purity and content of product.
Claims (10)
1. a kind of method of purification of sodium polydithio-dipropyl sulfonate, which is characterized in that be specially：It first will be poly- containing sodium sulfate salt
Two sulphur, two propane sulfonic acid mother liquid of sodium is successively by alkalescence anion-exchange resin, under the conditions of 30-60 DEG C under the conditions of 30-60 DEG C
Pass through acid cation exchange resin；Then regulation system pH value is to 3-7, successively by concentration, cooling, centrifugation, drying；Finally
Obtain high-purity sodium polydithio-dipropyl sulfonate.
2. the method for purification of sodium polydithio-dipropyl sulfonate as described in claim 1, which is characterized in that the polydithio-dipropyl
The content of sodium sulfate salt is 3-5% in sulfonic acid mother liquid of sodium, and the content of sodium polydithio-dipropyl sulfonate is 20-30%.
3. the method for purification of sodium polydithio-dipropyl sulfonate as claimed in claim 2, which is characterized in that described to contain sodium sulfate salt
Sodium polydithio-dipropyl sulfonate mother liquor be that our company's patent CN106946753A implements mother liquor obtained.
4. the method for purification of sodium polydithio-dipropyl sulfonate as described in claim 1, it is characterised in that：The alkali anion is handed over
Changing resin is macropore alkalinity acrylic acid type anion exchange resin, macropore basicity styrene series anion exchange resin or macropore benzene
One or more of ethylene system chelating ion exchange resin composition.
5. the method for purification of sodium polydithio-dipropyl sulfonate as claimed in claim 4, it is characterised in that：The alkali anion is handed over
Change resin be containing：
-N+(CH3)3The alkalescence anion-exchange resin of the comprehensive functional group of one or more of OH functional group.
6. the method for purification of sodium polydithio-dipropyl sulfonate according to claim 5, which is characterized in that the alkali anion
The dosage of exchanger resin is：The capacity of sulfate radical content and alkalescence anion-exchange resin ratio is 1:1-10.
7. the method for purification of sodium polydithio-dipropyl sulfonate as described in claim 1, it is characterised in that：The acid cation is handed over
Changing resin is one of macroreticular acidic acrylic acid type cation exchange resin, macroreticular acidic styrene type cation exchange resin
Or two kinds of compositions.
8. the method for purification of sodium polydithio-dipropyl sulfonate as claimed in claim 7, it is characterised in that：The acid cation is handed over
Change resin be containing：
The acid cation exchange resin of functional group.
9. the method for purification of sodium polydithio-dipropyl sulfonate according to claim 1, which is characterized in that the acid cation
Exchanger resin dosage is：The exchange capacity ratio of sodium polydithio-dipropyl sulfonate and the acid cation exchange resin is 1:1-
10。
10. the method for purification of sodium polydithio-dipropyl sulfonate according to claim 1, which is characterized in that described to pass through alkali
Before property anion exchange resin, the sodium polydithio-dipropyl sulfonate mother liquor containing sodium sulfate salt is first warming up to 45-60 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810835209.8A CN108912022A (en) | 2018-07-26 | 2018-07-26 | A kind of method of purification of sodium polydithio-dipropyl sulfonate |
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| CN201810835209.8A CN108912022A (en) | 2018-07-26 | 2018-07-26 | A kind of method of purification of sodium polydithio-dipropyl sulfonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113045459A (en) * | 2021-03-31 | 2021-06-29 | 潜江永安药业股份有限公司 | Method for removing sulfate radical in isethionate |
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| US6566552B2 (en) * | 1998-11-16 | 2003-05-20 | Sigma-Tau Industrie Farmaceutiche Riunite S.P.A. | Industrial process for the production of L-carnitine |
| WO2007139238A1 (en) * | 2006-05-26 | 2007-12-06 | Enzytech, Ltd. | Process for l-carnitine and acetyl l-carnitine hydrochloride |
| CN101519369A (en) * | 2009-04-03 | 2009-09-02 | 武汉中德远东精细化工有限公司 | Synthetic method of sodium polydithio-dipropyl sulfonate |
| CN106748934A (en) * | 2017-02-27 | 2017-05-31 | 江苏梦得新材料科技有限公司 | Desalting purifying devices and methods therefor in sodium polydithio-dipropyl sulfonate production process |
| CN106946753A (en) * | 2017-02-21 | 2017-07-14 | 湖北吉和昌化工科技有限公司 | The synthesis technique of sodium polydithio-dipropyl sulfonate |
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2018
- 2018-07-26 CN CN201810835209.8A patent/CN108912022A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| US6566552B2 (en) * | 1998-11-16 | 2003-05-20 | Sigma-Tau Industrie Farmaceutiche Riunite S.P.A. | Industrial process for the production of L-carnitine |
| WO2007139238A1 (en) * | 2006-05-26 | 2007-12-06 | Enzytech, Ltd. | Process for l-carnitine and acetyl l-carnitine hydrochloride |
| CN101519369A (en) * | 2009-04-03 | 2009-09-02 | 武汉中德远东精细化工有限公司 | Synthetic method of sodium polydithio-dipropyl sulfonate |
| CN106946753A (en) * | 2017-02-21 | 2017-07-14 | 湖北吉和昌化工科技有限公司 | The synthesis technique of sodium polydithio-dipropyl sulfonate |
| CN106748934A (en) * | 2017-02-27 | 2017-05-31 | 江苏梦得新材料科技有限公司 | Desalting purifying devices and methods therefor in sodium polydithio-dipropyl sulfonate production process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113045459A (en) * | 2021-03-31 | 2021-06-29 | 潜江永安药业股份有限公司 | Method for removing sulfate radical in isethionate |
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