CN109503647B - Process for preparing 3-isocyanatopropyltrimethoxysilane - Google Patents
Process for preparing 3-isocyanatopropyltrimethoxysilane Download PDFInfo
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- CN109503647B CN109503647B CN201710830163.6A CN201710830163A CN109503647B CN 109503647 B CN109503647 B CN 109503647B CN 201710830163 A CN201710830163 A CN 201710830163A CN 109503647 B CN109503647 B CN 109503647B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
Abstract
The invention discloses a preparation method of 3-isocyanate propyl trimethoxy silane with high conversion rate and without introducing a catalyst and an organic solvent, which comprises the following steps: the reaction device comprises a rectification column wound with an electric heating belt, wherein a kettle material receiving bottle is arranged at the bottom of the rectification column, a reflux discharge pipe of a distillation head at the top of the rectification column is communicated with a first receiving bottle, a connecting pipe of the distillation head is connected with a primary condensation pipe, the primary condensation pipe is communicated with a second receiving bottle, the second receiving bottle is connected with a secondary condensation pipe, the secondary condensation pipe is communicated with a third receiving bottle, the third receiving bottle is communicated with a third condensation pipe, and the third condensation pipe is communicated with a vacuum pump; secondly, controlling the temperature in a heating zone of the electric heating belt, a primary condensing pipe, a secondary condensing pipe and a tertiary condensing pipe, and controlling the vacuum degree in the reaction device; thirdly, dropwise adding raw material 3- (triethoxysilyl) propyl ] methyl carbamate, receiving the crude product in a first receiving bottle and a second receiving bottle, and receiving methanol in a third receiving bottle; and fourthly, carrying out vacuum rectification on the crude product to obtain the target product.
Description
Technical Field
The invention relates to a preparation method of 3-isocyanate propyl trimethoxy silane.
Background
3-isocyanatopropyltrimethoxysilane is a silane coupling agent containing an isocyanate reactive group and functions to promote the adhesion between inorganic materials and organic materials. It can be widely used for high-grade polyurethane sealant and modified polyurethane resin, and also can be used as a tackifier of room temperature vulcanized silicone rubber, a component of varnish resin and the like.
The following two methods are mainly used for synthesizing common isocyanato silane: firstly, dissolving carbamate in solvent, adding a certain amount of catalyst, cracking at high temperature, evaporating methanol generated by cracking in the reaction process, and then separating isocyanate from the kettle liquid. The first method has the disadvantages that: firstly, the addition of the solvent is not beneficial to the subsequent separation and purification. Secondly, the addition of the catalyst can catalyze the cracking but also cause the isocyanate polymerization, thereby reducing the yield. Second, an isocyanate compound is prepared by reacting phosgene with an amine in an inert solvent. The second method has the following disadvantages: phosgene is a colorless and tasteless highly toxic gas, and once the phosgene is leaked in the production process, serious safety accidents are easily caused.
Disclosure of Invention
The purpose of the invention is: provides a preparation method of 3-isocyanate propyl trimethoxy silane with high conversion rate, safety and convenience.
In order to achieve the purpose, the invention adopts the technical scheme that: the preparation process of 3-isocyanatopropyl trimethoxyl silane includes the following steps: a reaction apparatus is prepared, the reaction apparatus comprising: a rectification column with a filler inside, a feed inlet is arranged at the lower end part of the rectification column, an electric heating belt is wound on the rectification column below the feed inlet, a kettle material receiving bottle is connected to the bottom of the rectification column, a distillation head is connected to the top of the rectification column, the distillation head comprises a connecting pipe which is arranged obliquely upwards, a vertical downward backflow discharge pipe is arranged on the connecting pipe, the backflow discharge pipe is communicated with a first receiving bottle, a first-stage condensation pipe which is arranged obliquely upwards is connected to an outlet of the connecting pipe, a second receiving bottle is communicated with an outlet of the first-stage condensation pipe, the second receiving bottle is lower than the outlet of the first-stage condensation pipe, a second-stage condensation pipe is connected to the top of the second receiving bottle, a third receiving bottle is communicated with an outlet of the second-stage condensation pipe, the third receiving bottle is lower than the outlet of the second-stage condensation pipe, a third-stage condensation pipe is communicated with the top of the third-stage condensation pipe, and the condensation pipe is communicated with a vacuum pump, the outlet of each condensing pipe is higher than the inlet; secondly, controlling the temperature of a heating zone of the electric heating belt at 195-210 ℃, the temperature in a primary condensing tube at 75-90 ℃, the temperature in a secondary condensing tube at 55-65 ℃, the temperature in a tertiary condensing tube at-10-20 ℃, and the vacuum degree gauge pressure value in the reaction device at-0.08-0.09 Mpa; thirdly, dropwise adding raw material 3- (trimethoxysilyl) propyl methyl carbamate into the feeding hole, cracking the raw material in a rectifying column to generate gaseous 3-isocyanatopropyl trimethoxy silane and methanol, condensing and liquefying the gaseous 3-isocyanatopropyl trimethoxy silane in a primary condensing tube and a secondary condensing tube to reflux, receiving crude products in a first receiving bottle and a second receiving bottle, and condensing and liquefying the gaseous methanol in a tertiary condensing tube to reflux in a third receiving bottle; and fourthly, carrying out vacuum rectification on the crude products in the first receiving bottle and the second receiving bottle to obtain the target product 3-isocyanate propyl trimethoxy silane.
Further, in the preparation method of the 3-isocyanate propyl trimethoxy silane, the connecting pipe which is obliquely and upwards arranged is coaxial with the first-stage condensation pipe, and the included angle between the axis of the connecting pipe and the first-stage condensation pipe and the horizontal plane is 15-30 degrees.
Further, the preparation method of the 3-isocyanate propyl trimethoxy silane comprises the step of dropwise adding the raw materials into the rectifying column from the feed inlet by a peristaltic pump, wherein the dropwise adding speed of the raw materials is controlled to be 250 g/h-300 g/h.
Further, the preparation method of the 3-isocyanate propyl trimethoxy silane is characterized in that the gauge pressure value of the vacuum degree of the vacuum rectification in the fourth step is maintained at-0.1 Mpa, the kettle temperature during the vacuum rectification is not more than 135 ℃, and the temperature is raised to receive the fraction with the top temperature of 120 +/-3 ℃ so as to obtain the target product.
Further, in the preparation method of the 3-isocyanatopropyl-trimethoxysilane, the first-stage condenser pipe, the second-stage condenser pipe and the third-stage condenser pipe are all jacket-type condenser pipes, and condensing agents are introduced into the jackets of the first-stage condenser pipe, the second-stage condenser pipe and the third-stage condenser pipe.
Further, in the preparation method of the 3-isocyanatopropyltrimethoxysilane, before the raw materials are added, nitrogen is introduced from a feed inlet to exhaust oxygen in the reaction device.
Further, in the preparation method of the 3-isocyanatopropyl-trimethoxysilane, an outlet of the third-stage condensation pipe is communicated to a buffer bottle through a third tetrafluoroethylene hose, the buffer bottle is communicated with a vacuum pump through a fourth tetrafluoroethylene hose, and the buffer bottle is arranged lower than the third-stage condensation pipe.
Further, in the above method for preparing 3-isocyanatopropyltrimethoxysilane, the outlet of the primary condenser tube is connected with the second receiving bottle through the first tetrafluoroethylene hose, and the outlet of the secondary condenser tube is connected with the third receiving bottle through the second tetrafluoroethylene hose.
Further, in the preparation method of the 3-isocyanatopropyltrimethoxysilane, the distillation head also comprises a vertical connecting pipe, and a thermometer for monitoring the temperature in the distillation head is arranged on the vertical connecting pipe.
Further, in the preparation method of the 3-isocyanatopropyl trimethoxy silane, the filler in the rectifying column is a wire mesh filler or a glass spring filler.
The invention has the advantages that: the preparation method of the 3-isocyanate propyl trimethoxy silane has the advantages of high conversion rate, safety, convenience, no need of adding a catalyst and an organic solvent, few byproducts and low cost, can effectively separate the 3-isocyanate propyl trimethoxy silane from methane, and can be continuously carried out.
Drawings
FIG. 1 is a schematic view showing the structure of a reaction apparatus used in the process for preparing 3-isocyanatopropyltrimethoxysilane according to the invention.
Detailed Description
The preparation of 3-isocyanatopropyltrimethoxysilane is described in detail below.
The preparation process of 3-isocyanatopropyl trimethoxy silane includes the following steps.
First, a reaction apparatus is prepared, as shown in fig. 1, the reaction apparatus including: the inner part of the rectification column 1 is provided with a filler, and the filler in the rectification column 1 is a metal wire mesh filler or a glass spring filler. The lower end part of the rectifying column 1 is provided with a feeding hole 11, an electric heating belt 2 is wound on the rectifying column 1 below the feeding hole 11, the bottom of the rectifying column 1 is connected with a kettle material receiving bottle 3, the top of the rectifying column 1 is connected with a distillation head 4, the distillation head 4 comprises a vertical connecting pipe 42, and a thermometer 43 used for monitoring the temperature in the distillation head 4 is arranged on the vertical connecting pipe 42. The distillation head 4 further comprises a connecting pipe 41 which is obliquely arranged upwards, a backflow discharging pipe 44 which is vertically downwards is arranged on the connecting pipe 41, and the backflow discharging pipe 44 is communicated with the first receiving bottle 5. The exit linkage of connecting pipe 41 has the one-level condenser pipe 6 that the slope upwards set up, and the connecting pipe 41 that the slope upwards set up and the 6 coaxial lines of one-level condenser pipe, and connecting pipe 41 is 15 ~ 30 with the axis of one-level condenser pipe 6 and the contained angle theta of horizontal plane, and connecting pipe 41 upwards sets up with the slope of one-level condenser pipe 6 aim at: the gaseous 3-isocyanate propyl trimethoxy silane and the methanol can be effectively separated, and the side reaction caused by the contact of the gaseous 3-isocyanate propyl trimethoxy silane and the methanol is avoided, so that the yield can be greatly improved. The outlet of the primary condensation pipe 6 is communicated with a second receiving bottle 7, and specifically, the outlet of the primary condensation pipe 6 is communicated with the second receiving bottle 7 through a first tetrafluoroethylene hose 16. The second receiving bottle 7 is arranged below the outlet of the primary condensation pipe 6. The top of the second receiving bottle 7 is connected with a second-stage condensation pipe 8, an outlet of the second-stage condensation pipe 8 is communicated with a third receiving bottle 9, and specifically, an outlet of the second-stage condensation pipe 8 is communicated with the third receiving bottle 9 through a second tetrafluoroethylene hose 17. The third receiving bottle 9 is arranged below the outlet of the secondary condensation pipe 8. The top intercommunication of third receiving bottle 9 has tertiary condenser pipe 11, and tertiary condenser pipe 11 is linked together with vacuum pump 12, and the connection structure of tertiary condenser pipe 11 and vacuum pump 12 specifically includes: the outlet of the tertiary condenser pipe 11 is communicated to a buffer bottle 14 through a third tetrafluoroethylene hose 13, the buffer bottle 14 is communicated with a vacuum pump 12 through a fourth tetrafluoroethylene hose 15, and the buffer bottle 14 is lower than the outlet of the tertiary condenser pipe 11. The buffer vessel 14 is provided to effectively prevent material from being sucked into the vacuum pump 12. The outlet of each condensing pipe is higher than the inlet. The first-stage condenser pipe 6, the second-stage condenser pipe 8 and the third-stage condenser pipe 11 are all jacket type condenser pipes, condensing agents are introduced into jacket of the first-stage condenser pipe 6, the second-stage condenser pipe 8 and the third-stage condenser pipe 11, the condensing agents used by the first-stage condenser pipe 6 and the second-stage condenser pipe 8 are cooling water, and the condensing agents used by the third-stage condenser pipe 11 are refrigerating fluids.
Secondly, the temperature of the heating zone of the electric heating belt 2 is controlled to be 195-210 ℃, the temperature in the first-stage condensation pipe 6 is controlled to be 75-90 ℃, the temperature in the second-stage condensation pipe 8 is controlled to be 55-65 ℃, the temperature in the third-stage condensation pipe 11 is controlled to be-10-20 ℃, and the vacuum degree gauge pressure value in the reaction device is controlled to be-0.08 MPa-0.09 MPa.
And thirdly, before adding the raw materials, introducing nitrogen from the feed inlet 10 to exhaust oxygen in the reaction device. Then, the raw material 3- (trimethoxysilyl) propyl ] methyl carbamate was added dropwise from the feed inlet 10. Specifically, the raw materials are dripped into the rectification column 1 from the feed inlet 10 by a peristaltic pump, and the dripping speed of the raw materials is controlled to be 250 g/h-300 g/h. The raw materials are cracked and reacted in the rectifying column 1 to generate gaseous 3-isocyanate propyl trimethoxy silane and methanol, the gaseous 3-isocyanate propyl trimethoxy silane is condensed and liquefied and reflows in a primary condensation pipe 6 and a secondary condensation pipe 8, crude products are received in a first receiving bottle 5 and a second receiving bottle 7, and the gaseous methanol is condensed and liquefied and reflows in a tertiary condensation pipe 11 and is received in a third receiving bottle 9.
And fourthly, carrying out reduced pressure rectification on the crude products in the first receiving bottle 5 and the second receiving bottle 7, wherein the gauge pressure value of the vacuum degree is maintained at-0.1 Mpa during the reduced pressure rectification, the kettle temperature is not higher than 135 ℃ during the reduced pressure rectification, and the temperature is raised to receive the fraction with the top temperature of 120 +/-3 ℃ so as to obtain the target product 3-isocyanate propyl trimethoxy silane.
To further illustrate the preparation of 3-isocyanatopropyltrimethoxysilane, specific examples are given below.
Example 1.
Two tests were performed separately:
(1) the raw material is self-made 3- (trimethoxysilyl) propyl ] methyl carbamate (the purity is more than or equal to 90 percent, a small amount of 3-isocyanate propyl trimethoxy silane is contained, and the mass fraction is 7 percent) of 1024 g. Preparing a reaction device, heating the heating zone 2 to 202 ℃, introducing 80 ℃ cooling water into the jacket of the primary condenser pipe 6, introducing 60 ℃ cooling water into the jacket of the secondary condenser pipe 8, introducing-13 ℃ refrigerating fluid into the jacket of the tertiary condenser pipe 11, and controlling the vacuum degree gauge pressure value in the reaction device to be-0.085 Mpa. The nitrogen is replaced, the raw materials are conveyed from the feed inlet 10 by a peristaltic pump, and the dropping speed is controlled at 279 g/h. After the dropwise addition is finished, the materials in the kettle material receiving bottle 3 are: 32g, the total amount of the materials in the first receiving bottle 5 and the second receiving bottle 7 is as follows: 866g of crude product (3-isocyanatopropyltrimethoxysilane, 73% by weight), and 103g of product in a third receiver flask 9.
(2) The raw material is 1161g of self-made 3- (trimethoxysilyl) propyl ] methyl carbamate (the purity is more than or equal to 90 percent, and the mass fraction of the methyl carbamate contains a small amount of 3-isocyanatopropyl trimethoxy silane). Preparing a reaction device, heating the heating zone 2 to 198 ℃, introducing cooling water of 75 ℃ into a jacket of a primary condensing pipe 6, introducing cooling water of 65 ℃ into a jacket of a secondary condensing pipe 8, introducing refrigerating fluid of-12 ℃ into a jacket of a tertiary condensing pipe 11, and controlling the gauge pressure value of vacuum degree in the reaction device to be-0.087 Mpa. The nitrogen is replaced, the raw materials are conveyed from the feed inlet 10 by a peristaltic pump, and the dropping speed is controlled at 261 g/h. After the dropwise addition is finished, the materials in the kettle material receiving bottle 3 are: 43g, the total content of the materials in the first receiving bottle 5 and the second receiving bottle 7 is as follows: 958g of crude product (3-isocyanatopropyltrimethoxysilane, 75% by weight), and 129g of product in a third receiving flask 9.
And mixing the crude products obtained in the two tests, performing reduced pressure rectification, feeding 1823g (mass fraction of 74%) of the raw products after loss, maintaining the gauge pressure value of the vacuum degree at-0.1 Mpa during the reduced pressure rectification, controlling the kettle temperature at 135 ℃ at the maximum during the reduced pressure rectification, heating to receive fractions with the top temperature of 120 +/-3 ℃ to obtain 1213g (mass fraction of 96.3%) of the finished product 3-isocyanatopropyltrimethoxysilane and 595g of the kettle material.
The kettle charge was subjected to a continuous cracking test. Preparing a reaction device, heating the heating zone 2 to 193 ℃, introducing 90 ℃ cooling water into a jacket of a primary condensing pipe 6, introducing 55 ℃ cooling water into a jacket of a secondary condensing pipe 8, introducing-15 ℃ refrigerating fluid into a jacket of a tertiary condensing pipe 11, and controlling the vacuum degree gauge pressure value of the reaction device to be-0.087 Mpa. And (3) replacing nitrogen, namely conveying 590g (the purity is more than or equal to 85 percent, the content of a small amount of 3-isocyanate propyl trimethoxy silane is 10 percent) of the lost kettle material from a feed inlet 10 by a peristaltic pump, and controlling the dropping speed to be 254 g/h. After the dropwise addition is finished, the materials in the kettle material receiving bottle 3 are: 86g, the total amount of the materials in the first receiving bottle 5 and the second receiving bottle 7 is as follows: 414g of crude product (3-isocyanatopropyltrimethoxysilane, 80% by mass) and 65g of product in the third receiving flask 9. Crude 414g was mixed into the crude rectification of the next batch.
Example 2.
Two tests were performed separately:
(1) the raw material is 1355g of self-made 3- (trimethoxysilyl) propyl ] methyl carbamate (the purity is more than or equal to 90 percent, and the self-made methyl carbamate contains a small amount of 3-isocyanatopropyl trimethoxy silane, and the mass fraction is 7 percent). Preparing a reaction device, heating the heating zone 2 to 202 ℃, introducing cooling water of 85 ℃ into the jacket of the primary condenser pipe 6, introducing cooling water of 65 ℃ into the jacket of the secondary condenser pipe 8, introducing refrigerating fluid of-15 ℃ into the jacket of the tertiary condenser pipe 11, and controlling the gauge pressure value of vacuum degree in the reaction device to be-0.085 Mpa. The nitrogen is replaced, the raw materials are conveyed from the feed inlet 10 by a peristaltic pump, and the dropping speed is controlled at 288 g/h. After the dropwise addition is finished, the materials in the kettle material receiving bottle 3 are: 47g, the total amount of the materials in the first receiving bottle 5 and the second receiving bottle 7 is as follows: 1126g of crude product (3-isocyanatopropyltrimethoxysilane, 74% by mass) and 146g of product in a third receiving flask 9.
(2) The raw material is 1268g of self-made 3- (trimethoxysilyl) propyl ] methyl carbamate (the purity is more than or equal to 90 percent, and the mass fraction of the methyl carbamate contains a small amount of 3-isocyanatopropyl trimethoxy silane). Preparing a reaction device, heating the heating zone 2 to 208 ℃, introducing 80 ℃ cooling water into the jacket of the primary condenser pipe 6, introducing 60 ℃ cooling water into the jacket of the secondary condenser pipe 8, introducing-12 ℃ refrigerating fluid into the jacket of the tertiary condenser pipe 11, and controlling the vacuum degree gauge pressure value in the reaction device to be-0.082 Mpa. The nitrogen is replaced, the raw materials are conveyed from a feed inlet 10 through a peristaltic pump, and the dropping speed is controlled at 291 g/h. After the dropwise addition is finished, the materials in the kettle material receiving bottle 3 are: 85g, the total amount of the materials in the first receiving bottle 5 and the second receiving bottle 7 is as follows: 1006g of crude product (3-isocyanatopropyltrimethoxysilane, 75% by weight) and 136g of product in a third receiving flask 9.
Mixing the crude products obtained in the two tests, performing reduced pressure rectification, feeding 2128g (mass fraction of 74%) of the materials after loss, maintaining the gauge pressure value of vacuum degree at-0.1 Mpa during the reduced pressure rectification, controlling the maximum kettle temperature at 135 ℃ during the reduced pressure rectification, raising the temperature to receive fractions with the top temperature of 120 +/-3 ℃ to obtain 1416g (mass fraction of 96.7%) of the finished product 3-isocyanatopropyltrimethoxysilane and 637g of the kettle materials.
The kettle charge was subjected to a continuous cracking test. Preparing a reaction device, heating the heating zone 2 to 206 ℃, introducing cooling water of 75 ℃ into a jacket of a primary condensing pipe 6, introducing cooling water of 60 ℃ into a jacket of a secondary condensing pipe 8, introducing refrigerating fluid of-15 ℃ into a jacket of a tertiary condensing pipe 11, and controlling the vacuum degree gauge pressure value of the reaction device to be-0.083 Mpa. And (3) replacing nitrogen, namely conveying 635g (the purity is more than or equal to 85 percent, the mass fraction of the kettle material is 12 percent) of the lost kettle material from a feed inlet 10 by a peristaltic pump, and controlling the dropping speed at 295 g/h. After the dropwise addition is finished, the materials in the kettle material receiving bottle 3 are: 91g, the total amount of the materials in the first receiving bottle 5 and the second receiving bottle 7 is as follows: 440g of crude product (3-isocyanatopropyltrimethoxysilane, mass fraction 79%), and 68g of product in the third receiving flask 9. 440g of crude product is mixed into the next batch of crude product rectification.
From the above example, it is possible to obtain: the preparation method of the 3-isocyanate propyl trimethoxy silane has the advantages of high conversion rate, safety, convenience, no need of adding a catalyst and an organic solvent, few byproducts and low cost, can effectively separate the 3-isocyanate propyl trimethoxy silane from methane, and can be continuously carried out.
Claims (9)
- A process for preparing 3-isocyanatopropyltrimethoxysilane, comprising the steps of: a reaction apparatus is prepared, the reaction apparatus comprising: a rectification column with a filler inside, a feed inlet is arranged at the lower end part of the rectification column, an electric heating belt is wound on the rectification column below the feed inlet, a kettle material receiving bottle is connected at the bottom of the rectification column, a distillation head is connected at the top of the rectification column, the distillation head comprises a connecting pipe which is arranged obliquely upwards, a vertical downward backflow discharge pipe is arranged on the connecting pipe, the backflow discharge pipe is communicated with a first receiving bottle, a first-stage condensation pipe which is arranged obliquely upwards is connected to an outlet of the connecting pipe, the connecting pipe which is arranged obliquely upwards is coaxial with the first-stage condensation pipe, an included angle between the axis of the connecting pipe and the axis of the first-stage condensation pipe and a horizontal plane is 15-30 degrees, an outlet of the first-stage condensation pipe is communicated with a second receiving bottle, the second receiving bottle is lower than an outlet of the first-stage condensation pipe, the top of the second receiving bottle is connected with a second-stage condensation pipe, an outlet of the second-stage condensation pipe is communicated with a third receiving bottle, and the third receiving bottle is lower than an outlet of the second-stage condensation pipe, the top of the third receiving bottle is communicated with a third-stage condenser pipe, the third-stage condenser pipe is communicated with a vacuum pump, and an outlet of each condenser pipe is higher than an inlet; secondly, controlling the temperature of a heating zone of the electric heating belt at 195-210 ℃, the temperature in a primary condensing tube at 75-90 ℃, the temperature in a secondary condensing tube at 55-65 ℃, the temperature in a tertiary condensing tube at-10-20 ℃, and the vacuum degree gauge pressure value in the reaction device at-0.08-0.09 Mpa; thirdly, dropwise adding raw material 3- (trimethoxysilyl) propyl methyl carbamate into the feeding hole, cracking the raw material in a rectifying column to generate gaseous 3-isocyanatopropyl trimethoxy silane and methanol, condensing and liquefying the gaseous 3-isocyanatopropyl trimethoxy silane in a primary condensing tube and a secondary condensing tube to reflux, receiving crude products in a first receiving bottle and a second receiving bottle, and condensing and liquefying the gaseous methanol in a tertiary condensing tube to reflux in a third receiving bottle; and fourthly, carrying out vacuum rectification on the crude products in the first receiving bottle and the second receiving bottle to obtain the target product 3-isocyanate propyl trimethoxy silane.
- 2. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1, wherein: the raw materials are dripped into the rectifying column from the feed inlet by a peristaltic pump, and the dripping speed of the raw materials is controlled to be 250 g/h-300 g/h.
- 3. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: in the fourth step, the gauge pressure value of the vacuum degree of the vacuum rectification is maintained at-0.1 Mpa, the kettle temperature during the vacuum rectification is not more than 135 ℃, and the distillate with the top temperature of 120 +/-3 ℃ is received by heating, thus obtaining the target product.
- 4. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: the first-stage condenser pipe, the second-stage condenser pipe and the third-stage condenser pipe are all jacket type condenser pipes, and condensing agents are introduced into jacket of the first-stage condenser pipe, the second-stage condenser pipe and the third-stage condenser pipe.
- 5. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: before adding raw materials, nitrogen is firstly introduced from a feed inlet to exhaust oxygen in the reaction device.
- 6. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: the export of tertiary condenser pipe communicates to the buffer flask through the third tetrafluoroethylene hose, and the buffer flask is linked together through fourth tetrafluoroethylene hose and vacuum pump, the buffer flask be less than the setting of tertiary condenser pipe.
- 7. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: the outlet of the first-stage condensation pipe is communicated with the second receiving bottle through a first tetrafluoroethylene hose, and the outlet of the second-stage condensation pipe is communicated with the third receiving bottle through a second tetrafluoroethylene hose.
- 8. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: the distillation head also comprises a vertical connecting pipe, and a thermometer used for monitoring the temperature in the distillation head is arranged on the vertical connecting pipe.
- 9. A process for preparing 3-isocyanatopropyltrimethoxysilane according to claim 1 or 2, characterized in that: the packing in the rectification column is wire mesh packing or glass spring packing.
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3607901A (en) * | 1967-09-20 | 1971-09-21 | Gen Electric | Method of making isocyanatoalkyl-substituted silanes |
| US4064151A (en) * | 1976-05-17 | 1977-12-20 | United Carbide Corporation | Halosilyl carbamates |
| US5393910A (en) * | 1993-10-20 | 1995-02-28 | Osi Specialties, Inc. | Process for making isocyanatoorganosilanes |
| WO2005056565A1 (en) * | 2003-12-11 | 2005-06-23 | Consortium für elektrochemische Industrie GmbH | Method for the production of isocyanate organosilanes |
| CN1631893A (en) * | 2003-12-22 | 2005-06-29 | 张家港市国泰华荣化工新材料有限公司 | Process for preparing silicane containing isocyanate group |
| CN1839140A (en) * | 2003-12-11 | 2006-09-27 | 电化学工业有限公司（国际） | Method for producing isocyanate-organosilanes |
| CN101189246A (en) * | 2005-06-03 | 2008-05-28 | 莫门蒂夫功能性材料公司 | Process for the production of isocyanatosilane and silylisocyanurate |
| CN101307067A (en) * | 2007-05-16 | 2008-11-19 | 张家港市国泰华荣化工新材料有限公司 | Preparation method of isocyanate alkoxysilane |
| CN106488922A (en) * | 2014-07-14 | 2017-03-08 | 莫门蒂夫性能材料股份有限公司 | The manufacture method of the isocyanatoorganosilanes of low colourity and colour stable and derived from it product |
-
2017
- 2017-09-15 CN CN201710830163.6A patent/CN109503647B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3607901A (en) * | 1967-09-20 | 1971-09-21 | Gen Electric | Method of making isocyanatoalkyl-substituted silanes |
| US4064151A (en) * | 1976-05-17 | 1977-12-20 | United Carbide Corporation | Halosilyl carbamates |
| US5393910A (en) * | 1993-10-20 | 1995-02-28 | Osi Specialties, Inc. | Process for making isocyanatoorganosilanes |
| WO2005056565A1 (en) * | 2003-12-11 | 2005-06-23 | Consortium für elektrochemische Industrie GmbH | Method for the production of isocyanate organosilanes |
| CN1839140A (en) * | 2003-12-11 | 2006-09-27 | 电化学工业有限公司（国际） | Method for producing isocyanate-organosilanes |
| CN1631893A (en) * | 2003-12-22 | 2005-06-29 | 张家港市国泰华荣化工新材料有限公司 | Process for preparing silicane containing isocyanate group |
| CN101189246A (en) * | 2005-06-03 | 2008-05-28 | 莫门蒂夫功能性材料公司 | Process for the production of isocyanatosilane and silylisocyanurate |
| CN101307067A (en) * | 2007-05-16 | 2008-11-19 | 张家港市国泰华荣化工新材料有限公司 | Preparation method of isocyanate alkoxysilane |
| CN106488922A (en) * | 2014-07-14 | 2017-03-08 | 莫门蒂夫性能材料股份有限公司 | The manufacture method of the isocyanatoorganosilanes of low colourity and colour stable and derived from it product |
Non-Patent Citations (1)
| Title |
|---|
| 3-异氰酸丙基三乙氧基硅烷的合成研究;李淑辉等;《化学与黏合》;20170515(第03期);189-191页 * |
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