CN109824716A - A kind of recoverying and utilizing method of tributyltin chloride - Google Patents
A kind of recoverying and utilizing method of tributyltin chloride Download PDFInfo
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- CN109824716A CN109824716A CN201910189645.7A CN201910189645A CN109824716A CN 109824716 A CN109824716 A CN 109824716A CN 201910189645 A CN201910189645 A CN 201910189645A CN 109824716 A CN109824716 A CN 109824716A
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- tin
- monobutyl
- tributyltin chloride
- trichloride
- dichloride
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Abstract
The invention discloses a kind of recoverying and utilizing method of tributyltin chloride, include the following steps: that the tributyltin chloride of (1) by weight content less than 80% carries out high vacuum heating distillation in chlorination hydrogen atmosphere；Vacuum degree is 20Pa, and final warming temperature is 140 DEG C -160 DEG C；(2) the tributyltin chloride product obtained after vacuum distillation and tin tetrachloride mixed-controlled reaction thermotonus are obtained into the mixture of monobutyl-tin-trichloride and dibutyl tin dichloride；(3) mixture of monobutyl-tin-trichloride and dibutyl tin dichloride that step (2) obtains is subjected to distillation separation, respectively obtains monobutyl-tin-trichloride and dibutyl tin dichloride.Advantages of the present invention: final product monobutyl-tin-trichloride and dibutyl tin dichloride different melting points can be easily separated greatly, it produces useless few, it is easy to produce, and monobutyl-tin-trichloride and dibutyl tin dichloride can be used as individual product and use, and discarded tributyltin chloride catalyst is adequately recycled.
Description
Technical field
The present invention relates to organotin catalysts, in particular to a kind of recoverying and utilizing method of tributyltin chloride.
Background technique
Tributyltin chloride has the effects that anti-corrosion, sterilization, mould proof, makees rat poison, refuses in mouse cable coating and synthesis
Mesosome can be widely used for wood preservation, marine paints etc..It is widely used in pharmaceuticals industry as medicine intermediate simultaneously.It can use
Tributyl tin group and prostaglandin synthesis are imported in catalyst, organic synthesis.Tributyltin chloride is done in medicine processing
Between catalyst when can not continue to apply as waste since impurity content is higher after set uses certain number, and tributyl chlorine
It is serious to change tin environmental pollution, it is not easy to handle.
Summary of the invention
The technical problem to be solved in the present invention is to provide one kind can efficiently use discarded tributyltin chloride, reduction processing
The recoverying and utilizing method of the tributyltin chloride of cost pair.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows: a kind of recycling side of tributyltin chloride
Method includes the following steps: that the tributyltin chloride of (1) by weight content less than 80% carries out high vacuum liter in chlorination hydrogen atmosphere
Temperature distillation；Vacuum degree is 20Pa, and final warming temperature is 140 DEG C -160 DEG C；(2) the tributyl chlorination that will be obtained after vacuum distillation
Tin product and tin tetrachloride mixed-controlled reaction thermotonus obtain the mixing of monobutyl-tin-trichloride and dibutyl tin dichloride
Object；(3) mixture of monobutyl-tin-trichloride and dibutyl tin dichloride that step (2) obtains is subjected to distillation separation, respectively
Obtain monobutyl-tin-trichloride and dibutyl tin dichloride.
Further, the reaction temperature in the step (2) is 70-80 DEG C.
Further, the heating temperature in the step (2) is 75 degrees Celsius.
Further, monobutyl-tin-trichloride is the first fraction, and dibutyl tin dichloride is the second fraction, and described first evaporates
The recovered (distilled) temperature divided is 93 DEG C, and the recovered (distilled) temperature of second fraction is 41 DEG C.
Further, the final warming temperature in the step (1) is 150 DEG C.
By adopting the above technical scheme, due to by first carrying out rectification under vacuum to discarded tributyltin chloride catalyst, then
Monobutyl-tin-trichloride and dibutyl tin dichloride, monobutyl-tin-trichloride and dibutyl dichloro are generated simultaneously by single step reaction
Changing tin different melting points can be easily separated greatly, easy to produce, and monobutyl-tin-trichloride and dibutyl tin dichloride can be used as individually
Product uses, and generation waste is few, and discarded tributyltin chloride catalyst is adequately recycled.
Detailed description of the invention
Fig. 1 is the process flow chart in the present invention.
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing.It should be noted that for
The explanation of these embodiments is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, disclosed below
The each embodiment of the present invention involved in technical characteristic can be combined with each other as long as they do not conflict with each other.
Referring to Fig. 1, present embodiment discloses a kind of recoverying and utilizing method of tributyltin chloride, including walks as follows
Rapid: (1) tributyltin chloride by weight content less than 80% carries out high vacuum heating distillation in chlorination hydrogen atmosphere；Vacuum degree
For 20Pa, final warming temperature is 140 DEG C -160 DEG C；(2) the tributyltin chloride product and tetrachloro that will be obtained after vacuum distillation
Change tin mixed-controlled reaction thermotonus and obtains the mixture of monobutyl-tin-trichloride and dibutyl tin dichloride；(3) by step
(2) mixture of the monobutyl-tin-trichloride and dibutyl tin dichloride that obtain carries out distillation separation, respectively obtains monobutyl three
Stannic chloride and dibutyl tin dichloride.
Feasible, the reaction temperature in the step (2) is 70-80 DEG C.Preferably, the heating temperature in the step (2)
Degree is 75 degrees Celsius.
Wherein, the monobutyl-tin-trichloride in step (3) is the first fraction, and dibutyl tin dichloride is the second fraction, institute
The recovered (distilled) temperature for stating the first fraction is 93 DEG C, and the recovered (distilled) temperature of second fraction is 41 DEG C.It will be by a fraction point by fractionation
Out, distillating fraction is product.Due to by first carrying out rectification under vacuum to discarded tributyltin chloride catalyst, then pass through one
Monobutyl-tin-trichloride and dibutyl tin dichloride are reacted while being generated to step, and monobutyl-tin-trichloride and dibutyl tin dichloride are molten
Point difference can be easily separated greatly, easy to produce, and monobutyl-tin-trichloride and dibutyl tin dichloride can be used as individual product and make
With generation waste is few, and discarded tributyltin chloride catalyst is enabled adequately to be recycled.
For example, in this embodiment, specifically in the following way, the tributyl for being 80% by 41g weight content
Stannic chloride carries out high vacuum heating distillation in chlorination hydrogen atmosphere, using use for laboratory vacuum rectifying tower, is taken out using use for laboratory
Vacuum machine, setting vacuum degree are 20Pa, and final warming temperature is 150 DEG C；The tributyltin chloride obtained after vacuum distillation is produced
Object is put into reaction flask with 26g tin tetrachloride and is sufficiently mixed, and controls reaction temperature at 70-80 DEG C, reaction obtains monobutyl three
The mixture of stannic chloride and dibutyl tin dichloride；By the mixture of obtained monobutyl-tin-trichloride and dibutyl tin dichloride
Distillation separation is carried out, monobutyl-tin-trichloride and dibutyl tin dichloride are respectively obtained, the monobutyl-tin-trichloride finally obtained
Reach 98% with the purity of dibutyl tin dichloride.
In conjunction with attached drawing, the embodiments of the present invention are described in detail above, but the present invention is not limited to described implementations
Mode.For a person skilled in the art, in the case where not departing from the principle of the invention and spirit, to these embodiments
A variety of change, modification, replacement and modification are carried out, are still fallen in protection scope of the present invention.
Claims (5)
1. a kind of recoverying and utilizing method of tributyltin chloride, which comprises the steps of: (1) weight content is small
Tributyltin chloride in 80% carries out high vacuum heating distillation in chlorination hydrogen atmosphere；Vacuum degree is 20Pa, final heating temperature
Degree is 140 DEG C -160 DEG C；(2) by the tributyltin chloride product obtained after vacuum distillation and tin tetrachloride mixed-controlled reaction temperature
Degree reaction obtains the mixture of monobutyl-tin-trichloride and dibutyl tin dichloride；(3) the monobutyl trichlorine for obtaining step (2)
The mixture for changing tin and dibutyl tin dichloride carries out distillation separation, respectively obtains monobutyl-tin-trichloride and dibutyl dichloride
Tin.
2. a kind of recoverying and utilizing method of tributyltin chloride according to claim 1, which is characterized in that the step
(2) reaction temperature in is 70-80 DEG C.
3. a kind of recoverying and utilizing method of tributyltin chloride according to claim 2, which is characterized in that the step
(2) heating temperature in is 75 degrees Celsius.
4. a kind of recoverying and utilizing method of tributyltin chloride according to claim 1, which is characterized in that monobutyl trichlorine
Change tin is the first fraction, and dibutyl tin dichloride is the second fraction, and the recovered (distilled) temperature of first fraction is 93 DEG C, described second
The recovered (distilled) temperature of fraction is 41 DEG C.
5. a kind of recoverying and utilizing method of tributyltin chloride according to claim 1, which is characterized in that the step
(1) the final warming temperature in is 150 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910189645.7A CN109824716A (en) | 2019-03-13 | 2019-03-13 | A kind of recoverying and utilizing method of tributyltin chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910189645.7A CN109824716A (en) | 2019-03-13 | 2019-03-13 | A kind of recoverying and utilizing method of tributyltin chloride |
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| Publication Number | Publication Date |
|---|---|
| CN109824716A true CN109824716A (en) | 2019-05-31 |
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ID=66869175
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910189645.7A Pending CN109824716A (en) | 2019-03-13 | 2019-03-13 | A kind of recoverying and utilizing method of tributyltin chloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423248A (en) * | 2019-08-09 | 2019-11-08 | 南通名泰化工有限公司 | A kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride |
| EP4074717A1 (en) * | 2021-04-13 | 2022-10-19 | BNT Chemicals GmbH | Method for cleaving alkyl tin halides |
-
2019
- 2019-03-13 CN CN201910189645.7A patent/CN109824716A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110423248A (en) * | 2019-08-09 | 2019-11-08 | 南通名泰化工有限公司 | A kind of preparation method of high purity glass hot-end coating liquid monobutyl-tin-trichloride |
| EP4074717A1 (en) * | 2021-04-13 | 2022-10-19 | BNT Chemicals GmbH | Method for cleaving alkyl tin halides |
| US20220332735A1 (en) * | 2021-04-13 | 2022-10-20 | Bnt Chemicals Gmbh | Method for cleaving alkyl tin halides |
| US11912732B2 (en) * | 2021-04-13 | 2024-02-27 | Bnt Chemicals Gmbh | Method for cleaving alkyl tin halides |
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