CN103787373A - Method for purifying polysulfide silane coupling agent byproduct salt - Google Patents
Method for purifying polysulfide silane coupling agent byproduct salt Download PDFInfo
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- CN103787373A CN103787373A CN201410040228.3A CN201410040228A CN103787373A CN 103787373 A CN103787373 A CN 103787373A CN 201410040228 A CN201410040228 A CN 201410040228A CN 103787373 A CN103787373 A CN 103787373A
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Abstract
The invention aims at providing a method for purifying a polysulfide silane coupling agent byproduct salt. The method comprises the following steps: A, oxidizing sulfur ions, namely, feeding the byproduct saline of a polysulfide silane coupling agent into a reaction device, and adding a hydrogen peroxide solution in the stirring state to completely convert sulfur ions in the byproduct silane into sulfate radicals; and B, performing a hot saltpeter removal method, namely, filtering to remove impurities in the treated silane, performing multiple-effect evaporation on the obtained clear liquid so as to obtain byproducts sodium chloride and sodium sulfate. Whether the oxidation desulphuration ions are completely reacted can be detected by using a lead acetate test paper detection method or a copper chloride color change method. By adopting the method, sulfur ions can be completely converted into sulfate radicals, a sulfate product can be separated from sodium chloride by using the hot saltpeter removal method, and sodium chloride with high purity can be obtained. The problems of environment friendliness and purification treatment on the byproduct salt sodium chloride are solved.
Description
Technical field
The present invention relates to a kind of method that purifies polysulfide silanes coupling agent by-product salt, belong to chemical technology field.
Background technology
In the water production technique of polysulfide silanes coupling agent, having by product sodium-chlor to generate, is the form output with salt solution.Because organic chemical reactions can not 100% reacts completely and the generation of some side reactions, some unreacteds completely sulfonium ion remain in by-product salt solution, once touching sour environment, these sulfonium ions can be converted into toxic and harmful hydrogen sulfide, to environment, and likely personnel are damaged, and be unfavorable for that the further purification of by product sodium-chlor transforms.
At present domestic less than the relevant report to this by-product brine treatment, there is no a kind of ripe treatment process of the waste water for this kind of character.
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 that purifies polysulfide silanes coupling agent by-product salt solution, solved the purification process of environmental issue and by product sodium-chlor.
technical scheme: for achieving the above object, the present invention adopts following technical proposals:
A method that purifies polysulfide silanes coupling agent by-product salt, comprises the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, dripped hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are removed nitre: by above-mentioned brine filter removal of impurities after treatment, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
Whether completely above-mentioned oxidation sulphur removal ionic reaction detection method is the detection of use Lead acetate paper or cupric chloride variable color method.
beneficial effect: the present invention purifies polysulfide silanes coupling agent by-product salt solution alkalescence, that have sulfonium ion for product sodium-chlor except nitre operation by oxidation, hot method, efficiently solves the processing of polysulfide silanes coupling agent by-product salt.The inventive method can be converted into sulfate radical completely by sulfonium ion, and by hot method except the method for nitre separates vitriol product with sodium-chlor, obtain the sodium-chlor of higher degree.The environmental issue of polysulfide silanes coupling agent by-product salt solution and the purification process of by-product salt sodium-chlor are solved.
Embodiment
Below in conjunction with specific embodiment, the present invention is further described.
A method that purifies polysulfide silanes coupling agent by-product salt, comprises the steps:
A, sulfur oxide ion: the by-product salt solution of polysulfide silanes coupling agent is put in reaction unit, under whipped state, dripped hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are removed nitre: by above-mentioned brine filter removal of impurities after treatment, gained clear liquid carries out multiple-effect evaporation, obtains byproduct sodium-chlor and sodium sulfate.
Whether completely above-mentioned oxidation sulphur removal ionic reaction detection method is the detection of use Lead acetate paper or cupric chloride variable color method.
embodiment:
To the by-product salt solution that drops into two (propyl-triethoxysilicane) polysulfides of 3m3 in 5000L stirring tank, under whipped state, drip massfraction and be 27.5% hydrogen peroxide 30Kg, in dropping process, keep temperature of reaction system to be less than 90 ℃, dropping finishes rear stirring 15min to reacting completely, and stops stirring.From reaction system, getting about 50ml sample pours in Erlenmeyer flask, drip 1 dropper Cupric Chloride Solution in sample with 5mL Dispette, rock, produce precipitation, drip again hydrochloric acid to till recording the pH < 4 of sample with wide pH value test paper, if precipitation is not dissolved, reaction be described not exclusively, continue dropping hydrogen peroxide until sulfonium ion by complete oxidation; If being deposited in of producing drips after hydrochloric acid (the pH < 4 of sample) precipitation and disappear and show that sulfonium ion is by complete oxidation, reaction is reached home.Above-mentioned salt solution after treatment is crossed to pressure filter, remove impurity solid.Clear liquid is pumped into hot method except nitre multi-effect evaporation system, controlling an effect vaporization temperature is 90 ℃ ~ 100 ℃, two effect vaporization temperatures are controlled at 60 ℃ ~ 65 ℃, enter whizzer mother liquor temperature and be controlled at 45 ℃ ~ 50 ℃, whizzer solid is out product sodium-chlor, when after circulation for some time, mother liquor sampling survey sodium sulphate content reaches 61g/L left and right, mother liquor is entered to preheater preheating to be proceeded to and analyses nitre tank, the content of sodium sulfate is down to enter after 53g/L flash distillation further cooling concentrated after, enter again the evaporation of sodium-chlor salt cellar, operation so continuously, distill out respectively byproduct sodium-chlor and sodium sulfate.
The by-product salt of polysulfide silanes coupling agent water method production technique is to produce with aqueous solution form, and remaining unreacted sulfonium ion completely in this aqueous solution, may be converted into poisonous and hazardous hydrogen sulfide if deal with sulfonium ion improperly, causes environmental pollution and accident.The inventive method can be converted into sulfate radical completely by sulfonium ion, and vitriol product is separated with sodium-chlor except the method for nitre by hot method, thereby obtains the by-product salt solid sodium chloride of higher degree.The environmental issue of polysulfide silanes coupling agent by-product salt solution and the purification process of by-product salt sodium-chlor are solved.
Claims (2)
1. a method that purifies polysulfide silanes coupling agent by-product salt, 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, dripped hydrogen peroxide solution, the sulfonium ion in by-product salt solution is all converted into sulfate radical;
B, hot method are removed nitre: by above-mentioned brine filter removal of impurities after treatment, 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 according to claim 1, is characterized in that, whether completely oxidation sulphur removal ionic reaction detection method is the detection of use Lead acetate paper 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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| CN103787373A true CN103787373A (en) | 2014-05-14 |
| CN103787373B CN103787373B (en) | 2016-03-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467050A (en) * | 2018-06-07 | 2018-08-31 | 南京曙光精细化工有限公司 | A method of purification polysulfide silanes coupling agent by-product brine |
| CN108609634A (en) * | 2018-06-07 | 2018-10-02 | 南京曙光精细化工有限公司 | Continuous production purifies the device of polysulfide silanes coupling agent by-product brine |
| CN112300207A (en) * | 2020-11-19 | 2021-02-02 | 南京曙光精细化工有限公司 | Method for removing polysulfide silane coupling agent in byproduct saline |
| 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 |
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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 |
| WO2006124883A2 (en) * | 2005-05-12 | 2006-11-23 | Saudi Arabian Oil Company | Process of treating a spent caustic stream using an electrolyzer |
| 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 |
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Patent Citations (3)
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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 |
| WO2006124883A2 (en) * | 2005-05-12 | 2006-11-23 | Saudi Arabian Oil Company | Process of treating a spent caustic stream using an electrolyzer |
| 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)
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| 关汇川: ""过氧化氢在工业废水处理中的应用"", 《黎明化工》, no. 1, 31 December 1991 (1991-12-31), pages 8 - 11 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108467050A (en) * | 2018-06-07 | 2018-08-31 | 南京曙光精细化工有限公司 | A method of purification polysulfide silanes coupling agent by-product brine |
| CN108609634A (en) * | 2018-06-07 | 2018-10-02 | 南京曙光精细化工有限公司 | Continuous production purifies the device of polysulfide silanes coupling agent by-product brine |
| 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 |
| WO2021156085A1 (en) | 2020-02-06 | 2021-08-12 | Evonik Operations Gmbh | A process for the production of sulfur containing silanes by utilization of phase transfer catalysis |
| CN112300207A (en) * | 2020-11-19 | 2021-02-02 | 南京曙光精细化工有限公司 | Method for removing polysulfide silane coupling agent in byproduct saline |
| 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 |
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| CN103787373B (en) | 2016-03-02 |
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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. |