CN1763054A - Triphenyl stannic chloride raw material componemt, production method and uses - Google Patents
Triphenyl stannic chloride raw material componemt, production method and uses Download PDFInfo
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- CN1763054A CN1763054A CN 200510104258 CN200510104258A CN1763054A CN 1763054 A CN1763054 A CN 1763054A CN 200510104258 CN200510104258 CN 200510104258 CN 200510104258 A CN200510104258 A CN 200510104258A CN 1763054 A CN1763054 A CN 1763054A
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Abstract
The present invention relates to the material composition, production process and use of trichloro tin chloride, and belongs to the field of chemical technology. The production process includes the following steps: 1. xylene, metal sodium and chlorobenzene in certain weight proportion are reacted in no water, no oxygen and protective nitrogen condition; 2. adding the mixture of the rest chlorobenzene and tin tetrachloride; 3. reaction at 20-80 deg.c for 1-2 hr, adding aluminum trichloride, and reaction at 80-120 deg.c for 0.5-2.5 hr; 4. filtering; and 5. stirring, concentrating, cooling to 10-40 deg.c, letting stand for 1-3 hr and filtering to obtain product. The advantages includes improved material adding mode, shortened reaction time, reduced side reaction, high product yield, no sewage discharge, low material consumption, low cost and high production safety.
Description
One, belonging to the technical field
The invention relates to a raw material component of triphenyltin chloride, a production method and application thereof, belonging to the technical field of chemical product formulas and production methods.
Second, background Art
The prior art of the production method of the triphenyltin chloride, such as the large production technology of synthesizing the triphenyltin chloride by the Wutz method developed by the remote chemical industry headquarters, has the following problems: low yield, high cost, long reaction time, and the problems of pollution, flammability and even potential explosion of a small amount of waste water are not thoroughly solved.
Third, the invention
The invention aims to overcome the defects of the production method of the triphenyltin chloride in the prior art, and provides a triphenyltin chloride raw material component, a production method and application thereof, which have the advantages of high yield, low cost, short reaction time, no wastewater pollution and capability of thoroughly solving the problems of flammability and explosiveness.
The invention relates to a method for synthesizing triphenyl tin chloride by using a one-step method in an organic solvent under the action of a catalyst by taking active metal, benzene halide and tin tetrachloride as raw materials.
The technical solution of the invention is as follows:
the raw material components of the triphenyl tin chloride comprise active metal, benzene halide, tin tetrachloride, organic solvent and catalyst, wherein the active metal accounts for 0.8-1.5 parts by mass, the benzene halide accounts for 1-4 parts by mass, the tin tetrachloride accounts for 1-3 parts by mass, the organic solvent accounts for 1-8 parts by mass and the catalyst accounts for 0.03-0.1 part by mass;
the active metal comprises sodium Na, potassium K, magnesium Mg and the like; the halides of benzene include chlorobenzene, bromobenzene, iodobenzene, etc.; the organic solvent comprises toluene, xylene, petroleum ether and the like; the catalyst comprises metal chloride aluminum trichloride ALCL3Gallium trichloride GaCL3Calcium chloride CaCL2Etc.;
the invention relates to a method for producing triphenyl tin chloride,
1. under the protection conditions of no water, no oxygen and nitrogen, mixing 1-8 parts of organic solvent and 0.8-1.5 parts of active metal by mass, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the active metal at the stirring speed of 300 plus one 2500 rpm for 2-40 minutes to disperse the active metal into particles with the particle size of less than 120 mu m, and adding 0.02-0.1 part of benzene halide for primary initiation;
2. immediately cooling the dispersed material to 40-70 ℃ after the temperature rises to 2-3 ℃ after the first initiation, then adding the same amount of benzene halide for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of the total amount of 1-4 parts of benzene halide for full initiation, and then simultaneously mixing and adding the remaining benzene halide and 1-3 parts of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.03 to 0.1 portion of catalyst which is measured is added, and the temperatureis raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours;
4. filtering under 0.1-0.3Mpa via filter-pressing funnel to remove salt and catalyst;
5. putting the filter-pressed materials into a crystallization kettle, stirring, concentrating under 0.05-0.09Mpa, cooling to 10-40 deg.C, standing for 1-3 hr for crystallization, filtering in a filter tank to obtain the final product of triphenyltin chloride, drying, checking, and packaging.
The chemical reaction equation is as follows: (taking active metal sodium, benzene halide chlorobenzene, stannic chloride, organic solvent xylene, catalyst aluminum trichloride as examples),
the production method of the triphenyl tin chloride has a large amount of by-products of salt or salt residues;
the production method of the triphenyl tin chloride has the advantages that intermediate products are not separated, the hydrolysis procedure is removed, and the triphenyl tin chloride is directly converted into the triphenyl tin chloride through disproportionation;
the application of the triphenyl tin chloride of the invention is as follows: on the basis, the organic solvent adopts water or alcohols, and the triphenyl tin chloride is respectively mixed with NaOH and CH3COONa and NaF are used for respectively synthesizing triphenyl tin hydroxide, triphenyl tin acetate and triphenyl tin fluoride,
the synthesis of the triphenyl tin hydroxide is carried out,
synthesizing the triphenyl tin acetate to obtain the triphenyl tin acetate,
the synthesis of the triphenyl tin fluoride is carried out,
compared with the prior two-step method, the production method of the triphenyl tin chloride has the following technical advantages:
1. changing the feeding mode: the halobenzene and the stannic chloride are simultaneously mixed and added, so that the reaction time is shortened, the side reaction is reduced, and the yield is improved;
2. the generated tetraphenyltin is not separated, and is reacted with triphenyl tin chloride, diphenyl tin dichloride and the like which are generated simultaneously under the action of a catalyst; the hydrolysis procedure is cancelled, the sewage discharge is eliminated, the raw material consumption is reduced, and the process is a clean and pollution-free environment-friendly process;
3. the process adopts a one-step method, salt is recovered, the cost is reduced, and the production safety is improved;
4. the method for preparing the triphenyltin chloride has the advantages of simplest and simplest process, least three-waste discharge, safest production and highest yield.
Fourth, detailed description of the invention
Specific examples of the invention are given below:
example 1
The raw material components of triphenyltin chloride in this embodiment include active metal, benzene halide, tin tetrachloride, organic solvent, and catalyst, where in parts by mass, the active metal is 0.8 part, the benzene halide is 1 part, the tin tetrachloride is1 part, the organic solvent is 1 part, and the catalyst is 0.03 part;
the active metal comprises Na, K, Mg, etc.; the halides of benzene include chlorobenzene, bromobenzene, iodobenzene, etc.; the organic solvent comprises toluene, xylene, petroleum ether and the like; the catalyst packageIncludes metal chloride ALCL of aluminum trichloride3Gallium trichloride GaCL3Calcium chloride CaCL2Etc.;
the production method of triphenyltin chloride in this example is as follows:
in the production method of the following embodiment, active metal sodium, benzene halide chlorobenzene, organic solvent xylene, catalyst aluminum trichloride are taken as examples;
1. under the protection conditions of no water, no oxygen and nitrogen, 1 part of dimethylbenzene and 0.8 part of metallic sodium are put into a dispersion kettle according to the parts by mass, the kettle opening is sealed, jacket steam is opened to heat to 90-130 ℃, the metallic sodium is dispersed for 2-40 minutes by stirring at 300 plus 2500 rpm, the sodium is dispersed into particles with the particle size of less than 120 mu m, and 0.02 part of chlorobenzene is added for the first initiation;
2. when the temperature rises to 2-3 ℃, immediately cooling the dispersed material to 40-70 ℃, adding the same amount of chlorobenzene for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of 1 part of chlorobenzene in total for full initiation, transferring the material into a synthesis kettle, controlling the temperature to 10-30 ℃, and simultaneously mixing and adding the rest chlorobenzene and 1 part of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.03 part of metered aluminum trichloride is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours;
4. filtering under 0.1-0.3Mpa via filter-pressing funnel to remove salt and catalyst;
5. placing the filter-pressed material into a crystallization kettle, stirring, concentrating under 0.05-0.09Mpa negative pressure, cooling to 10-40 deg.C, standing for 1-3 hr for crystallization, discharging, filtering to obtain triphenyltin chloride product, drying, checking, and packaging;
the chemical reaction equation is as follows:
this example illustrates the use of triphenyltin chloride,
on the basis, the organic solvent is water or alcohol, triphenyl tin chloride is respectively mixed with NaOH and CH3COONa and NaF are used for respectively synthesizing triphenyl tin hydroxide, triphenyl tin acetate and triphenyl tin fluoride,
the synthesis of the triphenyl tin hydroxide is carried out,
synthesizing the triphenyl tin acetate to obtain the triphenyl tin acetate,
the synthesis of the triphenyl tin fluoride is carried out,
example 2 this example is a triphenyltin chloride which differs from example 1 in that,
the raw material components of triphenyltin chloride in this embodiment include active metal, benzene halide, tin tetrachloride, organic solvent, and catalyst, wherein in parts by mass, the active metal is 1.3 parts, the benzene halide is 4 parts, the tin tetrachloride is 3 parts, the organic solvent is 8 parts, and the catalyst is 0.1 part;
the method for producing triphenyltin chloride of this example is different from that of example 1 in that,
1. under the conditions of no water, no oxygen and nitrogen protection, mixing 8 parts of dimethylbenzene and 1.3 parts of metallic sodium by mass, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the metallic sodium at the stirring speed of 300-;
2. when the temperature rises to 2-3 ℃, immediately cooling the dispersed material to 40-70 ℃, adding the same amount of chlorobenzene for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of 4 parts of chlorobenzene in total for full initiation, and simultaneously mixing and adding the rest chlorobenzene and 3 parts of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.1 part of metered aluminum trichloride is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours.
Example 3 this example is a triphenyltin chloride which differs from example 1 in that,
the raw material components of triphenyltin chloride in this embodiment include, by mass, 1.0 part of an active metal, 2 parts of a benzene halide, 1.5 parts of tin tetrachloride, 2 parts of an organic solvent, and 0.05 part of a catalyst;
the method for producing triphenyltin chloride of this example is different from that of example 1 in that,
1. under the conditions of no water, no oxygen and nitrogen protection, mixing 2 parts of dimethylbenzene and 1.0 part of metallic sodium by mass, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the metallic sodium at the stirring speed of 300-2500 rpm for 2-40 minutes to disperse the sodium into particles with the particle size of less than 120 mu m, and adding 0.04 part of chlorobenzene to carry out primary initiation;
2. when the temperature rises to 2-3 ℃, immediately cooling the dispersed material to 40-70 ℃, adding the same amount of chlorobenzene for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of chlorobenzene in total in an amount of 2 parts, fully initiating, and simultaneously mixing and adding the rest chlorobenzene and 1.5 parts of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.05 part of metered aluminum trichloride is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours.
Example 4 this example is a triphenyltin chloride which differs from example 1 in that,
the raw material components of triphenyltin chloride in this embodiment include active metal, benzene halide, tin tetrachloride, organic solvent, and catalyst, wherein in parts by mass, the active metal is 1.2 parts, the benzene halide is 3 parts, the tin tetrachloride is 2.5 parts, the organic solvent is 4 parts, and the catalyst is 0.06 part;
the method for producing triphenyltin chloride of this example is different from that of example 1 in that,
1. under the conditions of no water, no oxygen and nitrogen protection, mixing 4 parts of dimethylbenzene and 1.2 parts of metallic sodium by mass, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the metallic sodium at the stirring speed of 300-2500 rpm for 2-40 minutes to disperse the sodium intoparticles with the particle size of less than 120 mu m, and adding 0.06 part of chlorobenzene to carry out primary initiation;
2. when the temperature rises to 2-3 ℃, immediately cooling the dispersed material to 40-70 ℃, adding the same amount of chlorobenzene for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of 3 parts of chlorobenzene in total for full initiation, and simultaneously mixing and adding the rest chlorobenzene and 2.5 parts of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.06 portion of aluminum trichloride which is measured is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours.
Example 5 this example is a triphenyltin chloride which differs from example 1 in that,
the raw material components of triphenyltin chloride in this embodiment include active metal, benzene halide, tin tetrachloride, organic solvent, and catalyst, wherein in parts by mass, the active metal is 1.5 parts, the benzene halide is 1.5 parts, the tin tetrachloride is 2 parts, the organic solvent is 6 parts, and the catalyst is 0.08 part;
the method for producing triphenyltin chloride of this example is different from that of example 1 in that,
1. under the conditions of no water, no oxygen and nitrogen protection, mixing 6 parts of dimethylbenzene and 1.5 parts of metallic sodium by mass, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the metallic sodium at the stirring speed of 300-;
2. when the temperature rises to 2-3 ℃, immediately cooling the dispersed material to 40-70 ℃, adding the same amount of chlorobenzene for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of 1.5 parts of chlorobenzene in total for full initiation, and simultaneously mixing and adding the rest chlorobenzene and 2 parts of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.08 part of metered aluminum trichloride is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours.
Example 6 this example is a triphenyltin chloride which differs from example 1 in that,
the raw material components of triphenyltin chloride in this embodiment include, by mass, 1.4 parts of active metal, 3.5 parts of benzene halide, 1.3 parts of tin tetrachloride, 7 parts of organic solvent, and 0.09 part of catalyst;
the method for producing triphenyltin chloride of this example is different from that of example 1 in that,
1. under the conditions of no water, no oxygen and nitrogen protection, mixing 7 parts of dimethylbenzene and 1.4 parts of metallic sodium by mass, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the metallic sodium at the stirring speed of 300-;
2. when the temperature rises to 2-3 ℃, immediately cooling the dispersed material to 40-70 ℃, adding the same amount of chlorobenzene for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of chlorobenzene in a total amount of 3.5 parts, fully initiating, and simultaneously mixing and adding the rest chlorobenzene and 1.3 parts of stannic chloride;
3. after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.09 part of aluminum trichloride is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours.
Compared with the existing two-step method technology, the above embodiment of the production method of the triphenyltin chloride can achieve the purpose of the invention, has the following technical advantages, and experiments and one-year trials prove that the production method of the triphenyltin chloride has stable effect and achieves the following advantages.
1. Changing the feeding mode: chlorobenzene and stannic chloride are simultaneously mixed and added, so that the reaction time is shortened, side reactions are reduced, and the yield is improved;
2. the generated tetraphenyltin is not separated, and is reacted with triphenyl tin chloride, diphenyl tin dichloride and the like which are generated simultaneously under the action of a catalyst; the hydrolysis procedure is cancelled, the sewage discharge is eliminated, the raw material consumption is reduced, and the process is a clean and pollution-free environment-friendly process;
3. the process adopts a one-step method, salt is recovered, the cost is reduced, and the production safety is improved;
4. the method for preparing the triphenyltin chloride has the advantages of simplest and simplest process, least three-waste discharge, safest production and highest yield.
Claims (8)
1. The raw material components of the triphenyl tin chloride are characterized in that: the catalyst comprises 0.8-1.5 parts of active metal, 1-4 parts of benzene halide, 1-3 parts of stannic chloride, 1-8 parts of organic solvent and 0.03-0.1 part of catalyst by mass.
2. A triphenyltin chloride starting material composition according to claim 1, wherein: the active metal comprises Na, K and Mg.
3. A triphenyltin chloride starting material composition according to claim 1, wherein: the benzene halide includes chlorobenzene, brominated benzene and iodinated benzene.
4. A triphenyltin chloride starting material composition according to claim 1, wherein: the organic solvent comprises toluene, xylene and petroleum ether.
5. A triphenyltin chloride starting material composition according to claim 1, wherein: the catalyst comprises metal chloride aluminum trichloride ALCL3Gallium trichloride GaCL3Calcium chloride CaCL2。
6. A process for producing triphenyltin chloride according to claim 1, wherein:
(1) under the protection conditions of no water, no oxygen and nitrogen, mixing 1-8 parts of organic solvent and 0.8-1.5 parts of active metal by mass part, adding the mixture into a dispersion kettle, heating to 90-130 ℃, stirring and dispersing the active metal at the stirring speed of 300-2500 rpm for 2-40 minutes to disperse the active metal into particles with the particle size of less than 120 mu m, and adding 0.02-0.1 part of benzene halide for primary initiation;
(2) immediately cooling the dispersed material to 40-70 ℃ after the first initiation when the temperature rises to 2-3 ℃, then adding the same amount of benzene halide for secondary initiation, quickly cooling to 10-30 ℃, dropwise adding 10-15% of the total amount of 1-4 parts of benzene halide for full initiation, and then simultaneously mixing and adding the remaining benzene halide and 1-3 parts of stannic chloride;
(3) after the addition, the temperature is between 20 and 80 ℃ for reaction for 1 to 2 hours, then 0.03 to 0.1 portion ofcatalyst which is measured is added, and the temperature is raised to between 80 and 120 ℃ for reaction for 0.5 to 2.5 hours;
(4) filtering under 0.1-0.3Mpa via filter-pressing funnel to remove salt and catalyst;
(5) placing the filter-pressed material into a crystallization kettle, stirring, concentrating under 0.05-0.09Mpa, cooling to 10-40 deg.C, standing for 1-3 hr for crystallization, filtering in a filter tank to obtain triphenyltin chloride product, drying, checking, packaging,
the chemical reaction equation is as follows:
7. a process for producing triphenyltin chloride according to claim 6, characterized in that: the intermediate product is not separated, the hydrolysis procedure is removed, and the intermediate product is directly disproportionated and converted into triphenyl tin chloride, and a large amount of by-product salt or salt residue is generated.
8. Use of triphenyltin chloride according to claim 1, wherein: on the basis, the organic solvent adopts water or alcohols, and the triphenyl tin chloride is respectively mixed with NaOH and CH3COONa and NaF are used for respectively synthesizing triphenyl tin hydroxide, triphenyl tin acetate and triphenyl tin fluoride,
the synthesis of the triphenyl tin hydroxide is carried out,
synthesizing the triphenyl tin acetate to obtain the triphenyl tin acetate,
the synthesis of the triphenyl tin fluoride is carried out,
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107915756A (en) * | 2017-12-07 | 2018-04-17 | 青岛天时化工有限公司 | The method for preparing triphenyl tin chloride |
| CN108002429A (en) * | 2017-12-05 | 2018-05-08 | 青岛天时化工有限公司 | The preparation process of butter of tin and triphenyl tin chloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1046528C (en) * | 1996-12-11 | 1999-11-17 | 双鸭山市光明精细化工厂 | Method for synthesizing triphenyl tin chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108002429A (en) * | 2017-12-05 | 2018-05-08 | 青岛天时化工有限公司 | The preparation process of butter of tin and triphenyl tin chloride |
| CN107915756A (en) * | 2017-12-07 | 2018-04-17 | 青岛天时化工有限公司 | The method for preparing triphenyl tin chloride |
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