CN102731556A - Process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane - Google Patents
Process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane Download PDFInfo
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- CN102731556A CN102731556A CN2012101871621A CN201210187162A CN102731556A CN 102731556 A CN102731556 A CN 102731556A CN 2012101871621 A CN2012101871621 A CN 2012101871621A CN 201210187162 A CN201210187162 A CN 201210187162A CN 102731556 A CN102731556 A CN 102731556A
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Abstract
The invention discloses a process for preparing tetramethyldivinyldisilazane by conversion of divinyl tetramethyl disiloxane. The process comprises steps of: (1) esterification reaction: first adding concentrated sulfuric acid into a dropping tank, and then adding thedivinyl tetramethyl disiloxane and petroleum benzene into a stirring kettle; then dropwise adding concentrated sulfuric acid into the stirring kettle, stopping stirring after reaction, releasing dilute sulfuric acid at the bottom upper, and introducing upper crude product into an ammoniation reactor; (2) ammoniation: opening a circulating water pump and mixing, opening an ammonia inlet valve, and introducing ammonia slowly; and (3) distillation: adding clear liquid into a rectification tower kettle, recovering petroleum benzene and intermediate distillate intermittently for recycling, and then recovering tetramethyldivinyldisilazane, so as to finally leave the target product of tetramethyldivinyldisilazane in the tower kettle. The process of the invention adopts a compressor recovery unit to carry out secondary amination synthesis and usage of ammonia, and avoids ammonia waste caused by the reaction pressure requirement.
Description
Technical field
The present invention relates to the preparation technology of tetramethyl divinyl disilazane, be specifically related to a kind of by tetramethyl divinyl disiloxane conversion tetramethyl divinyl disilazane preparation technology.
Background technology
At present domestic except that preparation technology with the synthetic tetramethyl divinyl disilazane of existing nothing temporarily the direct synthesis technique of raw material dimethyl-vinyl chlorosilane; This method greatest problem is the domestic no manufacturer of raw material dimethyl-vinyl chlorosilane, and the import difficulty is more and measure little.
Summary of the invention
The present invention is directed to the shortcoming in the background technology; Developed a kind of preparation technology who transforms tetramethyl divinyl disilazane by tetramethyl divinyl disiloxane; Little to solve the tetramethyl divinyl disilazane output that causes because of raw material is in short supply, to such an extent as to the too high problem of back step production cost.
Technical solution of the present invention:
Tetramethyl divinyl disiloxane transforms tetramethyl divinyl disilazane preparation technology, and concrete steps are:
1, esterification: at first in dripping jar, drop into the vitriol oil, in stirring tank, drop into tetramethyl divinyl disiloxane and petroleum benzene again, mix and stirred a hour; In stirring tank, drip the vitriol oil then, be added dropwise to complete in two hours, use the gas-liquid equilibrium device during reaction, temperature is controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 60 minutes is emitted the bottom dilute sulphuric acid, and the upper strata crude product is imported in the ammonification still;
2, ammonification: before ammonification, earlier bottom impurity is put only, into ammonia valve door is opened in ON cycle water pump and stirring then, slowly leads to ammonia, controlled temperature≤80 ℃, pressure≤0.18mpa.When the still temperature no longer rises, reach upper temperature limit and when beginning to descend, slowly close into ammonia valve, one hour no change of the nearly pressure high limit of still crimping gets into packing stage; When the reaction kettle temperature is higher than 1～2 ℃ of circulating water temperature, take out the washing of 1 bottle material earlier, add water again after the analysis confirmation of drawing a design reaction is thorough, material bag regular barrel is emitted the record analysis of checking the weight after washing twice.
3, rectifying: clear liquid is dropped in the rectifying tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction petroleum benzene (80 ℃ of cat head temperature) and middle distillate recycle; Extraction tetramethyl divinyl disiloxane (139 ℃ of cat head temperature) again, residue is purpose product tetramethyl divinyl disilazane (161 ℃ of top temperature) in the last tower still.
Said petroleum benzene: the vitriol oil: the tetramethyl divinyl disiloxane proportioning is 9～11:5～7:3～5.
The reaction formula that tetramethyl divinyl disiloxane conversion tetramethyl divinyl disilazane prepares in the process is:
1, main reaction:
2, side reaction:
Beneficial effect of the present invention:
The present invention adopts the compressor retrieving arrangement to utilize the ammonia secondary ammoniation is synthetic, has avoided wasting because of the ammonia that reaction pressure requires to cause, and has solved the pollution of ammonia emission to environment.Adopt potassium alcoholate, sodium alkoxide etc. not to produce the neutralizing agent of water in the N-process of the present invention, reaction is thorough, and the deposition of generation can be accumulated the after-filtration slagging-off.
Description of drawings
Accompanying drawing is a process flow diagram of the present invention.
Embodiment:
Below in conjunction with accompanying drawing and embodiment the present invention is further described.
Embodiment 1:
As shown in the figure, tetramethyl divinyl disiloxane transforms the tetramethyl divinyl disilazane step of preparation process and is:
1, esterification: at first in dripping jar, drop into the vitriol oil 1200 kg, in stirring tank, drop into tetramethyl divinyl disiloxane 800kg and petroleum benzene 2000kg again, mix and stirred a hour; In stirring tank, drip the vitriol oil then, be added dropwise to complete in two hours, use the gas-liquid equilibrium device during reaction, prevent benzene, tetramethyl divinyl disiloxane volatilization, not only reduced material loss, but also prevented that environmental pollution, temperature are controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 60 minutes is emitted the bottom dilute sulphuric acid, and the upper strata crude product is imported in the ammonification still;
2, ammonification: before ammonification, earlier bottom impurity is put only, into ammonia valve door is opened in ON cycle water pump and stirring then, slowly leads to ammonia, controlled temperature≤80 ℃, pressure≤0.18mpa.When the still temperature no longer rises, reach upper temperature limit and when beginning to descend, slowly close into ammonia valve, one hour no change of the nearly pressure high limit of still crimping gets into packing stage.When the reaction kettle temperature is higher than 1～2 ℃ of circulating water temperature, take out the washing of 1 bottle material earlier, add water again after the analysis confirmation of drawing a design reaction is thorough, material bag regular barrel is emitted the record analysis of checking the weight after washing twice.
3, rectifying: clear liquid is dropped in the rectifying tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction petroleum benzene (80 ℃ of cat head temperature) and middle distillate recycle; Extraction tetramethyl divinyl disiloxane cat head temperature is 139 ℃ again), residue is purpose product tetramethyl divinyl disilazane (161 ℃ of top temperature) in the last tower still.
Above-mentioned technology can prepare tetramethyl divinyl disilazane 751.2kg, and yield is 94.3%.
Embodiment 2:
As shown in the figure, tetramethyl divinyl disiloxane transforms the tetramethyl divinyl disilazane step of preparation process and is:
1, esterification: at first in dripping jar, drop into the vitriol oil 1000 kg, in stirring tank, drop into tetramethyl divinyl disiloxane 600kg and petroleum benzene 1800kg again, mix and stirred a hour; In stirring tank, drip the vitriol oil then, be added dropwise to complete in two hours, use the gas-liquid equilibrium device during reaction, prevent benzene, tetramethyl divinyl disiloxane volatilization, not only reduced material loss, but also prevented that environmental pollution, temperature are controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 60 minutes is emitted the bottom dilute sulphuric acid, and the upper strata crude product is imported in the ammonification still;
2, ammonification: before ammonification, earlier bottom impurity is put only, into ammonia valve door is opened in ON cycle water pump and stirring then, slowly leads to ammonia, controlled temperature≤80 ℃, pressure≤0.18mpa.When the still temperature no longer rises, reach upper temperature limit and when beginning to descend, slowly close into ammonia valve, one hour no change of the nearly pressure high limit of still crimping gets into packing stage.When the reaction kettle temperature is higher than 1～2 ℃ of circulating water temperature, take out the washing of 1 bottle material earlier, add water again after the analysis confirmation of drawing a design reaction is thorough, material bag regular barrel is emitted the record analysis of checking the weight after washing twice.
3, rectifying: clear liquid is dropped in the rectifying tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction petroleum benzene (80 ℃ of cat head temperature) and middle distillate recycle; Extraction tetramethyl divinyl disiloxane cat head temperature is 139 ℃ again), residue is purpose product tetramethyl divinyl disilazane (161 ℃ of top temperature) in the last tower still.
Above-mentioned technology can prepare tetramethyl divinyl disilazane 515.2kg, and yield is 92.3%.
Embodiment 3:
As shown in the figure, tetramethyl divinyl disiloxane transforms the tetramethyl divinyl disilazane step of preparation process and is:
1, esterification: at first in dripping jar, drop into the vitriol oil 1400 kg, in stirring tank, drop into tetramethyl divinyl disiloxane 1000kg and petroleum benzene 2200kg again, mix and stirred a hour; In stirring tank, drip the vitriol oil then, be added dropwise to complete in two hours, use the gas-liquid equilibrium device during reaction, prevent benzene, tetramethyl divinyl disiloxane volatilization, not only reduced material loss, but also prevented that environmental pollution, temperature are controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 60 minutes is emitted the bottom dilute sulphuric acid, and the upper strata crude product is imported in the ammonification still;
2, ammonification: before ammonification, earlier bottom impurity is put only, into ammonia valve door is opened in ON cycle water pump and stirring then, slowly leads to ammonia, controlled temperature≤80 ℃, pressure≤0.18mpa.When the still temperature no longer rises, reach upper temperature limit and when beginning to descend, slowly close into ammonia valve, one hour no change of the nearly pressure high limit of still crimping gets into packing stage.When the reaction kettle temperature is higher than 1～2 ℃ of circulating water temperature, take out the washing of 1 bottle material earlier, add water again after the analysis confirmation of drawing a design reaction is thorough, material bag regular barrel is emitted the record analysis of checking the weight after washing twice.
3, rectifying: clear liquid is dropped in the rectifying tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently extraction petroleum benzene (80 ℃ of cat head temperature) and middle distillate recycle; Extraction tetramethyl divinyl disiloxane cat head temperature is 139 ℃ again), residue is purpose product tetramethyl divinyl disilazane (161 ℃ of top temperature) in the last tower still.
Above-mentioned technology can prepare tetramethyl divinyl disilazane 953.6kg, and yield is 95.2%.
Claims (2)
1. tetramethyl divinyl disiloxane transforms the preparation technology of tetramethyl divinyl disilazane, and concrete steps are:
(1) esterification: at first in dripping jar, drop into the vitriol oil, in stirring tank, drop into tetramethyl divinyl disiloxane and petroleum benzene again, mix and stirred a hour; In stirring tank, drip the vitriol oil then, be added dropwise to complete in two hours, use the gas-liquid equilibrium device during reaction, temperature is controlled at below 60 ℃; Stop after reaction finishes stirring, static layering 60 minutes is emitted the bottom dilute sulphuric acid, and the upper strata crude product is imported in the ammonification still;
(2) ammonification: before ammonification, earlier bottom impurity is put only, into ammonia valve door is opened in ON cycle water pump and stirring then, slowly leads to ammonia, controlled temperature≤80 ℃, pressure≤0.18mpa; When the still temperature no longer rises, reach upper temperature limit and when beginning to descend, slowly close into ammonia valve, one hour no change of the nearly pressure high limit of still crimping gets into packing stage; When the reaction kettle temperature is higher than 1～2 ℃ of circulating water temperature, take out the washing of 1 bottle material earlier, add water again after the analysis confirmation of drawing a design reaction is thorough, material bag regular barrel is emitted the record analysis of checking the weight after washing twice;
(3) rectifying: clear liquid is dropped in the rectifying tower still; In 6～12 following varying reflux ratio operations of stage number; Intermittently the extraction petroleum benzene recycles with middle distillate, extraction tetramethyl divinyl disiloxane again, and residue is a purpose product tetramethyl divinyl disilazane in the last tower still.
2. tetramethyl divinyl disiloxane as claimed in claim 1 transforms the preparation technology of tetramethyl divinyl disilazane, and it is characterized in that: m-xylene in the above-mentioned steps: potassium metal: trimethylchlorosilane: the weight ratio of water is 4.5～5.5:0.8～1.2:2. 8～3.2:3～3.5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911198A (en) * | 2012-11-08 | 2013-02-06 | 广州市回天精细化工有限公司 | Hydroxyl scavenging compound and preparation method and purpose thereof |
| CN109867692A (en) * | 2017-12-01 | 2019-06-11 | 中昊晨光化工研究院有限公司 | A kind of preparation method of tetramethyl divinyl disilazane |
| CN111253429A (en) * | 2020-02-27 | 2020-06-09 | 聊城市鲁西化工工程设计有限责任公司 | Recycling device and method for organic silicon cracking high ring and application |
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| US6288132B1 (en) * | 2000-01-14 | 2001-09-11 | E. I. Du Pont De Nemours And Company | Organic gels |
| EP2028184A1 (en) * | 2007-08-21 | 2009-02-25 | Shin-Etsu Chemical Co., Ltd. | Method of producing organosilylamine containing radiation-polymerizable functional group and organosilylamine containing radiation-polymerizable functional group |
| CN101619071A (en) * | 2009-07-22 | 2010-01-06 | 吉林新亚强生物化工有限公司 | Preparation process of tetramethyl divinyl disilazane |
| CN101723964A (en) * | 2009-11-26 | 2010-06-09 | 浙江胡涂硅有限公司 | Preparation method of hexamethyl disilazane alkyl |
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2012
- 2012-06-08 CN CN2012101871621A patent/CN102731556A/en active Pending
Patent Citations (5)
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| JPH03261789A (en) * | 1990-03-12 | 1991-11-21 | Mitsui Toatsu Chem Inc | Production of silylamine |
| US6288132B1 (en) * | 2000-01-14 | 2001-09-11 | E. I. Du Pont De Nemours And Company | Organic gels |
| EP2028184A1 (en) * | 2007-08-21 | 2009-02-25 | Shin-Etsu Chemical Co., Ltd. | Method of producing organosilylamine containing radiation-polymerizable functional group and organosilylamine containing radiation-polymerizable functional group |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911198A (en) * | 2012-11-08 | 2013-02-06 | 广州市回天精细化工有限公司 | Hydroxyl scavenging compound and preparation method and purpose thereof |
| CN102911198B (en) * | 2012-11-08 | 2015-07-29 | 广州市回天精细化工有限公司 | A kind of hydroxyl removes compound, Its Preparation Method And Use |
| CN109867692A (en) * | 2017-12-01 | 2019-06-11 | 中昊晨光化工研究院有限公司 | A kind of preparation method of tetramethyl divinyl disilazane |
| CN111253429A (en) * | 2020-02-27 | 2020-06-09 | 聊城市鲁西化工工程设计有限责任公司 | Recycling device and method for organic silicon cracking high ring and application |
| CN111253429B (en) * | 2020-02-27 | 2023-06-27 | 聊城市鲁西化工工程设计有限责任公司 | Recycling device, method and application of organosilicon cracking high ring |
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Application publication date: 20121017 |