CN103787373B - The method of purification polysulfide silanes coupling agent by-product salt solution - Google Patents
The method of purification polysulfide silanes coupling agent by-product salt solution Download PDFInfo
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- CN103787373B CN103787373B CN201410040228.3A CN201410040228A CN103787373B CN 103787373 B CN103787373 B CN 103787373B CN 201410040228 A CN201410040228 A CN 201410040228A CN 103787373 B CN103787373 B CN 103787373B
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Abstract
The object of this invention is to provide a kind of method purifying polysulfide silanes coupling agent by-product salt solution, comprise the steps: A, sulfur oxide ion: put in reaction unit by the by-product salt solution of polysulfide silanes coupling agent, under whipped state, drip hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical; B, hot method are except nitre: by the brine filter removal of impurities after above-mentioned process, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.Wherein, the detection method whether sulfonium ion in by-product salt solution is all converted into sulfate radical is Lead acetate paper detection method or cupric chloride variable color method.Sulfonium ion can be converted into sulfate radical by the inventive method completely, and is separated with sodium-chlor by vitriol product by the method for hot method except nitre, obtains the sodium-chlor of higher degree.Solve the purification process of environmental issue and by-product salt sodium-chlor.
Description
Technical field
The present invention relates to a kind of method purifying polysulfide silanes coupling agent by-product salt solution, belong to chemical technology field.
Background technology
In the aqueous phase production technique of polysulfide silanes coupling agent, having side product chlorinated sodium to generate, is the form output with salt solution.Because organic chemical reactions can not 100% to react completely and the generation of some side reactions, some unreacteds completely sulfonium ion remain in by-product salt solution, these sulfonium ions can be converted into toxic and harmful hydrogen sulfide once touch sour environment, to environment, and likely personnel are damaged, and be unfavorable for that the further purification of side product chlorinated sodium transforms.
The domestic relevant report not to this by-product brine treatment, does not have a kind for the treatment of process of maturation of the waste water for this kind of character at present.
Summary of the invention
Goal of the invention: for solving the problems of the technologies described above, the object of this invention is to provide a kind of method purifying polysulfide silanes coupling agent by-product salt solution, solves the purification process of environmental issue and side product chlorinated sodium.
Technical scheme: for achieving the above object, the present invention adopts following technical proposals:
Purify a method for polysulfide silanes coupling agent by-product salt solution, comprise the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, drips hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are except nitre: by the brine filter removal of impurities after above-mentioned process, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
Wherein, the detection method whether sulfonium ion in by-product salt solution is all converted into sulfate radical is Lead acetate paper detection method or cupric chloride variable color method.
Beneficial effect: the present invention alkalescence, the polysulfide silanes coupling agent by-product salt solution that has sulfonium ion purified as product sodium-chlor except nitre operation by oxidation, hot method, efficiently solves the process of polysulfide silanes coupling agent by-product salt solution.Sulfonium ion can be converted into sulfate radical by the inventive method completely, and is separated with sodium-chlor by vitriol product by the method for hot method except nitre, obtains the sodium-chlor of higher degree.Solve the environmental issue of polysulfide silanes coupling agent by-product salt solution and the purification process of by-product salt sodium-chlor.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
Purify a method for polysulfide silanes coupling agent by-product salt solution, comprise the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, drips hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are except nitre: by the brine filter removal of impurities after above-mentioned process, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
Wherein, the detection method whether sulfonium ion in by-product salt solution is all converted into sulfate radical is Lead acetate paper detection method or cupric chloride variable color method.
Embodiment:
The by-product salt solution of two (propyl-triethoxysilicane) polysulfide of 3m3 is dropped in 5000L stirring tank, the hydrogen peroxide 30Kg that massfraction is 27.5% is dripped under whipped state, temperature of reaction system is kept to be less than 90 DEG C in dropping process, dropping terminates rear stirring 15min to reacting completely, and stops stirring.From reaction system, get about 50ml sample pours in Erlenmeyer flask, 1 dropper Cupric Chloride Solution is dripped in sample with 5mL Dispette, rock, produce precipitation, drip hydrochloric acid again to record the pH < 4 of sample with wide pH value test paper, if precipitation is not dissolved, illustrate that reaction not exclusively, continue to drip hydrogen peroxide until sulfonium ion is fully oxidized; If being deposited in of producing drips (the pH < 4 of sample) precipitation after hydrochloric acid and disappear, show that sulfonium ion is fully oxidized, reaction is reached home.Salt solution after above-mentioned process is crossed pressure filter, removing impurity solid.Clear liquid is pumped into hot method except nitre multi-effect evaporation system, controlling an effect vaporization temperature is 90 DEG C ~ 100 DEG C, two effect vaporization temperatures control at 60 DEG C ~ 65 DEG C, entering whizzer mother liquor temperature controls at 45 DEG C ~ 50 DEG C, whizzer solid is out product sodium-chlor, when after circulation for some time, mother liquor sampling survey sodium sulphate content reaches about 61g/L, mother liquor is entered preheater preheats to proceed to and analyse nitre tank, enter after making the content of sodium sulfate be down to 53g/L flash distillation lower the temperature further concentrated after, enter the evaporation of sodium-chlor salt cellar again, run so continuously, distill out byproduct sodium-chlor and sodium sulfate respectively.
The by-product salt of polysulfide silanes coupling agent Aqueous phase production technique produces as an aqueous solution, and remaining unreacted sulfonium ion completely in this aqueous solution, if deal with sulfonium ion improperly may be converted into poisonous and hazardous hydrogen sulfide, causes environmental pollution and accident.Sulfonium ion can be converted into sulfate radical by the inventive method completely, and is separated with sodium-chlor by vitriol product by the method for hot method except nitre, thus obtains the by-product salt solid sodium chloride of higher degree.Solve the environmental issue of polysulfide silanes coupling agent by-product salt solution and the purification process of by-product salt sodium-chlor.
Claims (2)
1. purify a method for polysulfide silanes coupling agent by-product salt solution, it is characterized in that comprising the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, drips hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are except nitre: by the brine filter removal of impurities after above-mentioned process, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
2. the method for purification polysulfide silanes coupling agent by-product salt solution according to claim 1, is characterized in that, the detection method whether sulfonium ion in by-product salt solution is all converted into sulfate radical is Lead acetate paper detection method or cupric chloride variable color method.
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| CN201410040228.3A CN103787373B (en) | 2014-01-28 | 2014-01-28 | The method of purification polysulfide silanes coupling agent by-product salt solution |
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| CN201410040228.3A CN103787373B (en) | 2014-01-28 | 2014-01-28 | The method of purification polysulfide silanes coupling agent by-product salt solution |
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| CN103787373A CN103787373A (en) | 2014-05-14 |
| CN103787373B true CN103787373B (en) | 2016-03-02 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467050B (en) * | 2018-06-07 | 2020-01-31 | 南京曙光精细化工有限公司 | method for purifying polysulfide silane coupling agent by-product brine |
| CN108609634B (en) * | 2018-06-07 | 2023-11-03 | 南京曙光新材料有限公司 | Device for purifying byproduct brine of polysulfide silane coupling agent in continuous production |
| EP3862358A1 (en) | 2020-02-06 | 2021-08-11 | Evonik Operations GmbH | A process for the production of sulfur containing silanes by utilization of phase transfer catalysis |
| CN112300207B (en) * | 2020-11-19 | 2024-01-30 | 南京曙光新材料有限公司 | Method for removing polysulfide silane coupling agent in byproduct brine |
Citations (2)
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|---|---|---|---|---|
| US4087253A (en) * | 1975-03-28 | 1978-05-02 | Rhone-Poulenc Industries | Method of obtaining caustic soda from a sodium chloride liquor containing sulphate ions recovered from an electrolytic cell |
| CN102633398A (en) * | 2011-02-12 | 2012-08-15 | 凯膜过滤技术(上海)有限公司 | Method for recovering organic effluent brine |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7713399B2 (en) * | 2005-05-12 | 2010-05-11 | Saudi Arabian Oil Company | Process for treating a sulfur-containing spent caustic refinery stream using a membrane electrolyzer powered by a fuel cell |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4087253A (en) * | 1975-03-28 | 1978-05-02 | Rhone-Poulenc Industries | Method of obtaining caustic soda from a sodium chloride liquor containing sulphate ions recovered from an electrolytic cell |
| CN102633398A (en) * | 2011-02-12 | 2012-08-15 | 凯膜过滤技术(上海)有限公司 | Method for recovering organic effluent brine |
Non-Patent Citations (2)
| Title |
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| "炼油厂加氢工艺废水的理论分析与综合治理";梁梓恒;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20131231(第S2期);B027-615正文第42页 * |
| "过氧化氢在工业废水处理中的应用";关汇川;《黎明化工》;19911231(第1期);第8-11页 * |
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Effective date of registration: 20160929 Address after: 210048 Jiangsu Province, Nanjing city of Nanjing Chemical Industrial Park Chongfu Road No. 226 Patentee after: NANJING SHUGUANG FINE CHEMICAL CO.,LTD. Address before: Yuhuatai District of Nanjing City, Jiangsu province 210041 Xi Shan Qiao Zhen Jia Dong Cun Youfang Bridge No. 136 Patentee before: NANJING SHUGUANG SILANE CHEMICAL Co.,Ltd. |
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Address after: No. 226 Chongfu Road, Nanjing Chemical Industry Park, Nanjing, Jiangsu Province, 210048 Patentee after: Nanjing Shuguang Fine Chemical Co.,Ltd. Address before: No. 226 Chongfu Road, Nanjing Chemical Industry Park, Nanjing, Jiangsu Province, 210048 Patentee before: NANJING SHUGUANG FINE CHEMICAL CO.,LTD. |
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