CN102516288B - The synthesis technique of dimethyltin chloride - Google Patents
The synthesis technique of dimethyltin chloride Download PDFInfo
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- CN102516288B CN102516288B CN201110373132.5A CN201110373132A CN102516288B CN 102516288 B CN102516288 B CN 102516288B CN 201110373132 A CN201110373132 A CN 201110373132A CN 102516288 B CN102516288 B CN 102516288B
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Abstract
The invention discloses a kind of synthesis technique of dimethyltin chloride, described synthesis technique comprises the steps: 1) tin, catalyzer and tin tetrachloride are joined in reactor, described catalyst charge is the 5-15% of tin weight, the add-on of described tin tetrachloride is the 1-10% of tin weight, is warming up to 160 DEG C-190 DEG C according to heating schedule; 2) control at 175-215 DEG C in temperature of reaction, reaction pressure controls at 0.5-1.5Mpa, stirs and add the methyl chloride gas of vaporization in described reactor, until reaction terminates; 3) after reaction terminates, control at 180-250 DEG C in temperature of reaction, reaction pressure controls at 1.3-1.5Mpa, insulation reaction 2-4 hour, by the obtained dimethyltin chloride of distillation after insulation terminates.The present invention has obtained a kind of high purity dimethyl tindichloride, and improves the method for tin slab utilization ratio and methyl chloride tin yield, and the method adopts high-pressure process one step to catalyze and synthesize, and technique is simple, and generated time is short, and product purity is high.
Description
Technical field
Invention relates to the production field of fine chemistry industry, more specifically, and the particularly synthesis technique of high purity dimethyl tindichloride.
Background technology
Dimethyltin chloride (DMTC), English name: Dimethyltin Dichloride, CAS NO:753-73-1, molecular formula: C
2h
6cl
2sn, relative molecular mass: 219.57.
The dimethyltin chloride being mixed with tin methyltrichloride, mainly for the production of methyl tin heat stabilizer, is the main raw material producing methyl tin heat stabilizer; But highly purified dimethyltin chloride is along with development scientific and technical in recent years, it suppresses for magnesium or alloy corrosion, and LOW-E glass coating, the association areas such as esterification catalytic increase year by year.And use on LOW-E glass coating and have unrivaled superiority.
Not only technique is loaded down with trivial details for traditional method preparing dimethyltin chloride, and severe reaction conditions, and yield is low.Most domestic producer all improves its production technique, and such as the normal preparation technology adopted is one-step synthesis at present.But mostly adopt the reaction of 500L small-sized reactor in the process, its long reaction time and the purity of dimethyltin chloride is not high, due to reaction conditions, cause tin slab utilization ratio to only have about 92%.
The existing publication number that patent discloses is 101921290A, denomination of invention is the patent of a kind of preparation method of dimethyltin chloride, a kind of preparation method of dimethyltin chloride of this disclosure of the invention, it comprises the following steps: 1) be the tin of 1: 0.1 ~ 0.5: 0.1 ~ 0.3, catalyzer and tin tetrachloride by weight ratio, be warmed up to 100 ~ 170 DEG C in confined conditions, described catalyzer is tetramethyl ammonium chloride or tetrabutylammonium chloride; 2) under whipped state, add methyl chloride, continue to be warming up to 170 ~ 250 DEG C, pressure is 0.9 ~ 1.7MPa, stops adding the follow-up continuous stirring of methyl chloride 1 ~ 5 hour, the dimethyltin chloride of obtained gaseous state; 3) the temperature of gaseous state dimethyltin chloride be 180 ~ 260 DEG C, under pressure is 0.9 ~ 1.7MPa, adopt and use water as absorption liquid and carry out falling film absorption, soak time is 1 ~ 6 hour, the obtained dimethyltin chloride aqueous solution.
But aforesaid method complex process, the product produced is the mixture of monomethyl tin trichloride and dimethyltin chloride, be unsuitable for producing highly purified dimethyltin chloride and having many by products after using catalyzer, and, the large danger of current this method temperature of reaction high pressure is large, product yield is not high, and has environmental pollution, and industrialization is produced and application to cause current method to be unfavorable for like this.
Summary of the invention
The object of the invention is to the deficiency overcoming above-mentioned existence, the object of the present invention is to provide a kind of synthesis technique of high purity dimethyl tindichloride, and improve the method for tin slab utilization ratio and methyl chloride tin yield, the method adopts high-pressure process one step to catalyze and synthesize, technique is simple, generated time is short, and product purity is high.
Technical scheme of the present invention is as follows:
Technical problem to be solved by this invention is: a kind of synthesis technique of dimethyltin chloride, and described synthesis technique comprises the steps:
1) join in reactor by tin, catalyzer and tin tetrachloride, described catalyst charge is the 5-15% of tin weight, and the add-on of described tin tetrachloride is the 1-10% of tin weight, is warming up to 160 DEG C-190 DEG C according to heating schedule;
2) control at 175-215 DEG C in temperature of reaction, reaction pressure controls at 0.5-1.5Mpa, stirs and add the methyl chloride gas of vaporization in described reactor, until reaction terminates;
3) after reaction terminates, control at 180-250 DEG C in temperature of reaction, reaction pressure controls at 1.3-1.5Mpa, insulation reaction 2--4 hour, by the obtained dimethyltin chloride of distillation after insulation terminates.
Another aspect of the present invention, in described step 1, catalyzer is dimethyl sulfoxide (DMSO) or dimethyl sulphide, and add-on is the 8%-15% of tin weight.
Another aspect of the present invention, in described step 1, catalyst charge is 10% of tin weight.
Another aspect of the present invention, in described step 1, heating schedule is that per minute heats up 1 DEG C-8 DEG C.
Another aspect of the present invention, in described step 1, heating schedule is that per minute heats up 1.5 DEG C.
Another aspect of the present invention, the temperature of reaction in described step 2 controls at 180-210 DEG C, and reaction pressure controls at 0.9-1.3Mpa, reaction times 2-4 hour.
Another aspect of the present invention, the temperature of reaction in described step 3 controls at 200-240 DEG C, and reaction pressure controls at 1.3-1.5Mpa, reaction times 2-4 hour.
Another aspect of the present invention, the add-on of described step 1 tin tetrachloride is the 1-4% of tin weight.
Another aspect of the present invention, the Theil indices of the tin slab in described step 3 is more than 99.95%.
Another aspect of the present invention, in air distillation in described step 3, and receives the cut of gas reactor temperature between 188 DEG C-200 DEG C.
Beneficial effect of the present invention is: the present invention discloses a kind of preparation method of high purity dimethyl tindichloride, and improving the method for tin slab utilization ratio and methyl chloride tin yield, the method adopts high-pressure process one step to catalyze and synthesize, and technique is simple, generated time is short, and product purity is high.
The present invention not only changes the method for grignard reagent legal system in the past for dimethyltin chloride, also shorten the reaction times prepared by single stage method, not only purity is good for obtained dimethyltin chloride, yield is high, and catalyzer only needs to add and once can recycle more than 50 times, tin slab utilization ratio can reach more than 96%.
Embodiment
Embodiment 1
Special agitator is being housed, thermometer, in the pressure reaction still of tensimeter and conduit, add tin grain 300 kilograms, dimethyl sulfoxide (DMSO) 30 kilograms, tin tetrachloride 10 kilograms, solid dimethyltin chloride 200 kilograms, 180 DEG C are warming up to according to heat-up rate 1.5 DEG C/min, between the pressure 0.9-1.3Mpa of control methyl chloride, about reaction 4 hours, control temperature of reaction at 180-210 DEG C, the consumption of methyl chloride is at about 300 kilograms, reaction terminates, then temperature of reaction is controlled at 200-240 DEG C, pressure 1.3-1.5Mpa, react about 2h, then air distillation, and receive the cut of gas reactor temperature between 188 DEG C-200 DEG C, obtained dimethyltin chloride.The utilization ratio of tin slab is 96.5%; The yield 98.9% of methyl tin, wherein dimethyltin chloride accounts for 98.7%, tin methyltrichloride 1.2%, trimethyltin chloride 0.1%, Contents of Main Components 99% in dimethyltin chloride solid after distillation.
Embodiment 2
Special agitator is being housed, thermometer, in the pressure reaction still of tensimeter and conduit, add tin grain 350 kilograms, dimethyl sulfoxide (DMSO) 5 kilograms, tin tetrachloride 10 kilograms, solid dimethyltin chloride in example 1 and distillation at the end of remaining black solid slag charge totally 250 kilograms, 188 DEG C are warming up to according to heat-up rate 2 DEG C/min, control temperature of reaction at 180-210 DEG C, between the pressure 0.9-1.3Mpa of control methyl chloride, about reaction 4 hours, control temperature of reaction at 180-210 DEG C, the consumption of methyl chloride is at about 350 kilograms, reaction terminates, then temperature of reaction is controlled at 200-240 DEG C, pressure 1.3-1.5Mpa, react about 2h, then air distillation, and receive the cut of gas reactor temperature between 188 DEG C-200 DEG C, obtained dimethyltin chloride.The utilization ratio of tin slab is 95.5%; The yield 98.1% of methyl tin, wherein dimethyltin chloride accounts for 98.9%, tin methyltrichloride 1.0%, trimethyltin chloride 0.1%, Contents of Main Components 99% in dimethyltin chloride solid after distillation.
Embodiment 3
Special agitator is being housed, thermometer, in the pressure reaction still of tensimeter and conduit, add tin grain 250 kilograms, dimethyl thioether 30 kilograms, tin tetrachloride 10 kilograms, in example 2 receive solid dimethyltin chloride and distillation at the end of remaining black solid slag charge totally 200 kilograms, 180 DEG C are warming up to according to heat-up rate 1.0 DEG C/min, between the pressure 0.9-1.3Mpa of control methyl chloride, about reaction 4 hours, control temperature of reaction at 180-210 DEG C, the consumption of methyl chloride is at about 250 kilograms, reaction terminates, then temperature of reaction is controlled at 200-240 DEG C, pressure 1.3-1.5Mpa, react about 2h, then air distillation, and receive the cut of gas reactor temperature between 188 DEG C-200 DEG C, obtained dimethyltin chloride.The utilization ratio of tin slab is 97.1%; The yield 99.0% of methyl tin, wherein dimethyltin chloride accounts for 98.7%, tin methyltrichloride 1.2%, trimethyltin chloride 0.1%, Contents of Main Components 99% in dimethyltin chloride solid after distillation.
Embodiment 4
Special agitator is being housed, thermometer, in the pressure reaction still of tensimeter and conduit, add tin grain 250 kilograms, dimethyl thioether 1 kilogram, tin tetrachloride 3 kilograms, solid dimethyltin chloride in example 3 and distillation at the end of remaining black solid slag charge totally 200 kilograms, 180 DEG C are warming up to according to heat-up rate 1.5 DEG C/min, between the pressure 1.1-1.4Mpa of control methyl chloride, about reaction 4 hours, control temperature of reaction at 180-210 DEG C, the consumption of methyl chloride is at about 250 kilograms, reaction terminates, then temperature of reaction is controlled at 200-240 DEG C, pressure 1.3-1.5Mpa, react about 2h, then air distillation, and receive the cut of gas reactor temperature between 188 DEG C-200 DEG C, obtained dimethyltin chloride.The utilization ratio of tin slab is 97.9%; The yield 99.1% of methyl tin, wherein dimethyltin chloride accounts for 99.2%, tin methyltrichloride 0.7%, trimethyltin chloride 0.1%, Contents of Main Components 99% in dimethyltin chloride solid after distillation.
Embodiment 5
Special agitator is being housed, thermometer, in the pressure reaction still of tensimeter and conduit, add tin grain 300 kilograms, dimethyl thioether 1 kilogram, tin tetrachloride 5 kilograms, solid dimethyltin chloride in example 4 and distillation at the end of remaining black solid slag charge totally 250 kilograms, 180 DEG C are warming up to according to heat-up rate 1.5 DEG C/min, between the pressure 1.1-1.3Mpa of control methyl chloride, about reaction 4 hours, control temperature of reaction at 180-210 DEG C, the consumption of methyl chloride is at about 300 kilograms, reaction terminates, then temperature of reaction is controlled at 200-240 DEG C, pressure 1.3-1.5Mpa, react about 2h, then air distillation, and receive the cut of gas reactor temperature between 188 DEG C-200 DEG C, obtained dimethyltin chloride.The utilization ratio of tin slab is 97.9%; The yield 99.1% of methyl tin, wherein dimethyltin chloride accounts for 99.3%, tin methyltrichloride 0.7%, trimethyltin chloride 0.1%, Contents of Main Components 99% in dimethyltin chloride solid after distillation.
Embodiment 6
Special agitator is being housed, thermometer, in the pressure reaction still of tensimeter and conduit, add tin grain 300 kilograms, dimethyl sulfoxide (DMSO) 2 kilograms, tin tetrachloride 5 kilograms, solid dimethyltin chloride in example 5 and distillation at the end of remaining black solid slag charge totally 250 kilograms, 180 DEG C are warming up to according to heat-up rate 1.5 DEG C/min, between the pressure 1.1-1.3Mpa of control methyl chloride, about reaction 4 hours, control temperature of reaction at 180-210 DEG C, the consumption of methyl chloride is at about 300 kilograms, reaction terminates, then temperature of reaction is controlled at 200-240 DEG C, pressure 1.3-1.5Mpa, react about 2h, then air distillation, and receive the cut of gas reactor temperature between 188 DEG C-200 DEG C, obtained dimethyltin chloride.The utilization ratio of tin slab is 97.1%; The yield 98.6% of methyl tin, wherein dimethyltin chloride accounts for 98.3%, tin methyltrichloride 1.6%, trimethyltin chloride 0.1%, Contents of Main Components 99% in dimethyltin chloride solid after distillation.
So far invention has been described in conjunction with the embodiments.Those skilled in the art should be appreciated that without departing from the scope and spirit of the present invention, easily can make other amendment various to described embodiment.Therefore, the scope of appended claims is not limited to above-mentioned explanation, but broadly will explain claim.
Claims (8)
1. a synthesis technique for dimethyltin chloride, is characterized in that: described synthesis technique comprises the steps:
1) tin, catalyzer and tin tetrachloride are joined in reactor, described catalyst charge is the 5-15% of tin weight, the add-on of described tin tetrachloride is the 1-10% of tin weight, 160 DEG C-190 DEG C are warming up to according to heating schedule, described catalyzer is dimethyl sulphide or DMSO, and described heating schedule is that per minute heats up 1 DEG C-8 DEG C;
2) control at 175-215 DEG C in temperature of reaction, reaction pressure controls at 0.5-1.5Mpa, stirs and add the methyl chloride gas of vaporization in described reactor, until reaction terminates;
3) after reaction terminates, control at 180-250 DEG C in temperature of reaction, reaction pressure controls at 1.3-1.5Mpa, insulation reaction 2--4 hour, by the obtained dimethyltin chloride of distillation after insulation terminates, described distillation in air distillation, and receives gas reactor temperature at the cut of 188 DEG C-200 DEG C.
2. the synthesis technique of dimethyltin chloride according to claim 1, is characterized in that: in described step 1, catalyst charge is the 8%-15% of tin weight.
3. the synthesis technique of dimethyltin chloride according to claim 2, is characterized in that: in described step 1, catalyst charge is 10% of tin weight.
4. the synthesis technique of dimethyltin chloride according to claim 1, is characterized in that: in described step 1, heating schedule is that per minute heats up 1.5 DEG C.
5. the synthesis technique of dimethyltin chloride according to claim 1, is characterized in that: the temperature of reaction in described step 2 controls at 180-210 DEG C, and reaction pressure controls at 0.9-1.3Mpa, reaction times 2-4 hour.
6. the synthesis technique of dimethyltin chloride according to claim 1, is characterized in that: the temperature of reaction in described step 3 controls at 200-240 DEG C, and reaction pressure controls at 1.3-1.5Mpa, reaction times 2-4 hour.
7. the synthesis technique of dimethyltin chloride according to claim 1, is characterized in that: the add-on of described tin tetrachloride is the 1-4% of tin weight.
8. the synthesis technique of dimethyltin chloride according to claim 1, is characterized in that: the Theil indices of the tin slab in described step 3 is more than 99.95%.
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| CN201110373132.5A CN102516288B (en) | 2011-11-22 | 2011-11-22 | The synthesis technique of dimethyltin chloride |
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| CN201110373132.5A CN102516288B (en) | 2011-11-22 | 2011-11-22 | The synthesis technique of dimethyltin chloride |
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| CN107089678A (en) * | 2017-05-26 | 2017-08-25 | 南通艾德旺化工有限公司 | A kind of preparation method and applications of butter of tin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077196A (en) * | 1992-08-13 | 1993-10-13 | 北京科技协作中心精细化学分部 | Preparation of a mixture of dimethyltin dichloride and methyltrichlorotin |
| CN1117495A (en) * | 1994-08-24 | 1996-02-28 | 深圳泛胜塑胶助剂有限公司 | Tin methide Stabilizer, the prepn. thereof |
| CN101838283A (en) * | 2009-12-29 | 2010-09-22 | 衢州建华东旭助剂有限公司 | Production method of high-purity dimethyltin dichloride crystal |
| CN101921290A (en) * | 2010-07-28 | 2010-12-22 | 潍坊益华化工有限公司 | Method for preparing dimethyltin chloride |
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2011
- 2011-11-22 CN CN201110373132.5A patent/CN102516288B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1077196A (en) * | 1992-08-13 | 1993-10-13 | 北京科技协作中心精细化学分部 | Preparation of a mixture of dimethyltin dichloride and methyltrichlorotin |
| CN1117495A (en) * | 1994-08-24 | 1996-02-28 | 深圳泛胜塑胶助剂有限公司 | Tin methide Stabilizer, the prepn. thereof |
| CN101838283A (en) * | 2009-12-29 | 2010-09-22 | 衢州建华东旭助剂有限公司 | Production method of high-purity dimethyltin dichloride crystal |
| CN101921290A (en) * | 2010-07-28 | 2010-12-22 | 潍坊益华化工有限公司 | Method for preparing dimethyltin chloride |
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Effective date of registration: 20210820 Address after: 226200 Hezuo Shihai Town, Qidong City, Nantong City, Jiangsu Province Patentee after: Qidong Qiangqiang Trade Co.,Ltd. Address before: 226221 Yanjiang fine chemical park, Beixin Town, Qidong City, Jiangsu Province Patentee before: NANTONG ADVANCE CHEMICALS Co.,Ltd. |
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