CN113896892A - Method for continuously producing polysiloxane - Google Patents
Method for continuously producing polysiloxane Download PDFInfo
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- CN113896892A CN113896892A CN202111109324.5A CN202111109324A CN113896892A CN 113896892 A CN113896892 A CN 113896892A CN 202111109324 A CN202111109324 A CN 202111109324A CN 113896892 A CN113896892 A CN 113896892A
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- -1 polysiloxane Polymers 0.000 title claims abstract description 90
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 68
- 238000000034 method Methods 0.000 title claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 33
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 27
- 150000001336 alkenes Chemical class 0.000 claims abstract description 27
- 229920000570 polyether Polymers 0.000 claims abstract description 27
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims abstract description 16
- 229920001577 copolymer Polymers 0.000 claims abstract description 10
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 15
- BITPLIXHRASDQB-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane Chemical compound C=C[Si](C)(C)O[Si](C)(C)C=C BITPLIXHRASDQB-UHFFFAOYSA-N 0.000 claims description 15
- 229910052697 platinum Inorganic materials 0.000 claims description 15
- 238000010924 continuous production Methods 0.000 claims description 6
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- ZQJAONQEOXOVNR-UHFFFAOYSA-N n,n-di(nonyl)nonan-1-amine Chemical compound CCCCCCCCCN(CCCCCCCCC)CCCCCCCCC ZQJAONQEOXOVNR-UHFFFAOYSA-N 0.000 claims description 3
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 3
- 239000000047 product Substances 0.000 description 36
- 238000003756 stirring Methods 0.000 description 16
- 239000012855 volatile organic compound Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- IUMSDRXLFWAGNT-UHFFFAOYSA-N Dodecamethylcyclohexasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 IUMSDRXLFWAGNT-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/32—Post-polymerisation treatment
- C08G77/34—Purification
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention provides a method for continuously producing polysiloxane, which comprises the following steps: continuously adding hydrosiloxane, polyether or olefin and catalyst solution into at least one series of continuous stirred tank reactors to mix; discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last continuous stirred tank reactor; the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300 rpm; adding a terminator to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product; pre-devolatilizing the polysiloxane mixed product in a falling strip devolatilizer; the pre-devolatilized polysiloxane mixed product is subjected to secondary enhanced devolatilization in a double-screw extruder to obtain polysiloxane.
Description
Technical Field
The invention relates to the technical field of polysiloxane production, in particular to a method for continuously producing polysiloxane.
Background
The synthesis of the ultrahigh viscosity polysiloxane mostly adopts a catalytic equilibrium process, and the used equipment is a polymerization kettle. In order to obtain polysiloxane with ultra-high viscosity, the production is generally realized by prolonging the polymerization time and the developping time. After the reaction is finished, 12 to 15 percent of Volatile Organic Compounds (VOCs) such as octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane (D5), dodecamethylcyclohexasiloxane (D6) and the like exist, and need to be removed.
The existing method for preparing the polysiloxane with ultrahigh viscosity is complex, and the prepared polysiloxane has insufficient viscosity and more content of the volatile organic compounds at the back in the preparation process.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for continuously producing polysiloxane, which has the advantages of simple preparation mode, easy operation, and capability of obtaining polysiloxane with higher viscosity and lower volatile component.
The above object of the present invention is achieved by the following technical solutions: a method for the continuous production of polysiloxanes, comprising the steps of:
step 1: continuously adding hydrogen siloxane, polyether or olefin and catalyst solution into at least one series of continuous stirring tank reactors for mixing;
step 2: discharging a mixture comprising the siloxane copolymer and unreacted hydrosiloxane and the olefin or polyether from the outlet of the last continuous stirred tank reactor;
and step 3: the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300 rpm;
and 4, step 4: adding a terminator to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
and 5: pre-devolatilizing the polysiloxane mixed product in a falling strip devolatilizer;
step 6: and carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain the polysiloxane.
Preferably, the catalyst is a platinum complex of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane.
Preferably, the mixing temperature is 170-190 ℃.
Preferably, the terminating agent is selected from one of diethylamine, tri-n-butylamine, trinonyl amine and silazane.
Preferably, the temperature of the pre-devolatilization is 140-160 ℃, and the vacuum degree of the pre-devolatilization is 60-100 Pa.
In summary, the invention includes at least one of the following beneficial technical effects:
1. the hydrogen siloxane, polyether or olefin and the catalyst solution are mixed, and a plurality of continuous stirring tank reactors are arranged for stirring, so that the three can react to the maximum extent, and the mixture can be remotely conveyed through the continuous stirring tank reactors, so that the equipment can be conveniently matched.
2. The reaction was more complete by adding the mixture to a continuous mixer and shearing the mixture through 2 dissolver disks to allow the constituent components of the mixture to further fuse with each other.
3. Through carrying out both sides intensive devolatilization to the polysiloxane mixed product, make the volatile organic compound in the mixed product obtain further processing, avoid the volatile substance in the polysiloxane finished product to account for the proportion height, further promote the performance of product to the viscosity of the polysiloxane that adopts this application step 1 to step 6 to prepare is high, volatile organic compound accounts for the ratio low, has improved the nature of product, and the preparation method is simple moreover, easily operates.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present application clearer, the technical solutions of the embodiments of the present application will be clearly and completely described below. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the application without any inventive step, are within the scope of protection of the application.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this application belongs. The use of the terms "a" or "an" and the like in the description and in the claims of the present application do not denote a limitation of quantity, but rather denote the presence of at least one.
The invention relates to a method for continuously producing polysiloxane, which comprises the following steps:
step 1: add hydrogen siloxane, polyether or alkene and catalyst solution to at least one series of continuous stirred tank reactor continously and mix, this application adopts two series of continuous stirred tank reactors to prepare, makes different continuous stirred tank reactors can carry out abundant stirring to the composition that adds, makes and fuses each other between the composition, the progress of the later stage process of being convenient for.
In the application, the added catalyst is a platinum complex of chloroplatinic acid and 1, 3-divinyl tetramethyl disiloxane, the market supply is sufficient, the price is low, the industrial batch production can be realized, and the catalyst can play a role of catalysis to the greatest extent and is convenient for reaction among the components.
In the application, the mixing temperature of the components is 170-190 ℃, the mixing efficiency can be accelerated, and the time required by mixing is reduced.
Step 2: and discharging the mixture containing the siloxane copolymer, unreacted hydrosiloxane and olefin or polyether from the outlet of the last continuous stirring tank reactor, and communicating the outlet with the inlet of the continuous mixer, so that the mixture is convenient to transport, a series of operations such as transportation and the like are avoided, time and labor are saved, and the reaction is more sufficient.
In the present application, the stirring rate of the continuous stirring tank reactor is 100 to 500rpm, and more specifically, the stirring rate of the continuous stirring tank reactor is 150rpm, 300rpm or 400 rpm.
And step 3: the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300 rpm; through shearing and mixing, the components for reaction in the mixture can contact each other to the maximum extent to abundant reaction that reacts, its reaction effect is better, moreover, the shearing angle and the speed of steerable splice tray, more further make and react between the mixture. The reaction efficiency is improved.
And 4, step 4: adding a terminator to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product; the invention is promoted to obtain the crude product of the ultra-high viscosity polysiloxane by stopping the reaction in the continuous mixer by adding a terminating agent, wherein the terminating agent is selected from one of diethylamine, tri-n-butylamine, trinonyl amine and silazane.
And 5: pre-devolatilizing the obtained ultra-high viscosity polysiloxane mixed product in a falling strip devolatilizer; namely, the ultra-high viscosity polysiloxane mixed product is subjected to preliminary devolatilization, so that the content of volatile organic compounds is preliminarily reduced, and the quality of the product is further improved.
Step 6: and (3) performing secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, and matching the polysiloxane with the falling strip devolatilizer in the step (5) to form a two-layer devolatilization structure, so that the mixture is subjected to devolatilization twice, the content of volatile organic compounds is further reduced, and the quality of the product is further improved.
In the prior art, the devolatilization method is mainly carried out in a falling bar type devolatilizer, but the viscosity of the product is gradually increased along with the volatilization of volatile organic compounds in the product and the reduction of the amount of residual monomers, so that the devolatilization is more and more difficult, therefore, the whole process is carried out under high vacuum so as to reduce the partial pressure of volatile components in a gas phase as much as possible, so that the prepared product has ultrahigh content of volatile organic compounds, and the quality of the product is influenced.
In this application, in order to improve productivity, can also through increase melt specific surface area and improvement surface renewal rate, thereby increase the diffusion rate of volatile components in the fuse-element and improve reaction rate, further quickening reaction rate improves work efficiency.
In the present application, all amounts and percentage data in the examples are based on weight and all pressures are 0.10MPa (abs.), unless otherwise stated.
Example 1:
1) continuously adding hydrogen siloxane, polyether or olefin and platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane into a first series of continuous stirred tank reactors for mixing, wherein the stirring speed is 150rpm, the feeding amount of hydrogen siloxane is 100kg/h, the feeding amount of polyether or olefin is 0.3kg/h, the feeding amount of platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane is 0.03kg/h, and the mixing temperature is 170 ℃;
2) discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last series of continuous stirred tank reactors;
3) the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300rpm for 2 h;
4) adding diethylamine with the feeding amount of 0.03kg/h to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
5) discharging the polysiloxane mixed product into a falling strip devolatilizer for pre-devolatilization; the pre-devolatilization temperature is 140 ℃, and the vacuum degree is 60 Pa;
6) and finally, carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, wherein the temperature of a screw barrel is 200 ℃, the vacuum degree is 30Pa, and the rotating speed of the screw is 105rp, and finally obtaining the polysiloxane with ultrahigh viscosity and ultralow volatility.
Example 2:
1) continuously adding hydrogen siloxane, polyether or olefin and platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane into a first series of continuous stirred tank reactors for mixing, wherein the stirring speed is 150rpm, the feeding amount of the hydrogen siloxane is 95kg/h, the feeding amount of the polyether or olefin is 0.3kg/h, the feeding amount of the platinum complex solution of the chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane is 0.03kg/h, and the mixing temperature is 170 ℃;
2) discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last series of continuous stirred tank reactors;
3) the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300rpm for 2 h;
4) adding diethylamine with the feeding amount of 0.03kg/h to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
5) discharging the polysiloxane mixed product into a falling strip devolatilizer for pre-devolatilization; the pre-devolatilization temperature is 140 ℃, and the vacuum degree is 60 Pa;
6) and finally, carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, wherein the temperature of a screw barrel is 200 ℃, the vacuum degree is 30Pa, and the rotating speed of the screw is 105rp, and finally obtaining the polysiloxane with ultrahigh viscosity and ultralow volatility.
Example 3:
1) continuously adding hydrogen siloxane, polyether or olefin and platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane into a first series of continuous stirred tank reactors for mixing, wherein the stirring speed is 150rpm, the feeding amount of the hydrogen siloxane is 90kg/h, the feeding amount of the polyether or olefin is 0.3kg/h, the feeding amount of the platinum complex solution of the chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane is 0.03kg/h, and the mixing temperature is 170 ℃;
2) discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last series of continuous stirred tank reactors;
3) the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300rpm for 2 h;
4) adding diethylamine with the feeding amount of 0.03kg/h to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
5) discharging the polysiloxane mixed product into a falling strip devolatilizer for pre-devolatilization; the pre-devolatilization temperature is 140 ℃, and the vacuum degree is 60 Pa;
6) and finally, carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, wherein the temperature of a screw barrel is 200 ℃, the vacuum degree is 30Pa, and the rotating speed of the screw is 105rp, and finally obtaining the polysiloxane with ultrahigh viscosity and ultralow volatility.
Example 4:
1) continuously adding hydrogen siloxane, polyether or olefin and platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane into a first series of continuous stirred tank reactors for mixing, wherein the stirring speed is 150rpm, the feeding amount of the hydrogen siloxane is 100kg/h, the feeding amount of the polyether or olefin is 0.3kg/h, the feeding amount of the platinum complex solution of the chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane is 0.03kg/h, and the mixing temperature is 170 ℃;
2) discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last series of continuous stirred tank reactors;
3) the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300rpm for 2 h;
4) adding silazane in a feeding amount of 0.03kg/h to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
5) discharging the polysiloxane mixed product into a falling strip devolatilizer for pre-devolatilization; the pre-devolatilization temperature is 140 ℃, and the vacuum degree is 60 Pa;
6) and finally, carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, wherein the temperature of a screw barrel is 200 ℃, the vacuum degree is 30Pa, and the rotating speed of the screw is 105rp, and finally obtaining the polysiloxane with ultrahigh viscosity and ultralow volatility.
Example 5:
1) continuously adding hydrogen siloxane, polyether or olefin and platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane into a first series of continuous stirred tank reactors for mixing, wherein the stirring speed is 150rpm, the feeding amount of the hydrogen siloxane is 100kg/h, the feeding amount of the polyether or olefin is 0.3kg/h, the feeding amount of the platinum complex solution of the chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane is 0.03kg/h, and the mixing temperature is 170 ℃;
2) discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last series of continuous stirred tank reactors;
3) the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300rpm for 2 h;
4) adding silazane in a feeding amount of 0.03kg/h to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
5) discharging the polysiloxane mixed product into a falling strip devolatilizer for pre-devolatilization; the pre-devolatilization temperature is 150 ℃, and the vacuum degree is 70 Pa;
6) and finally, carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, wherein the temperature of a screw barrel is 200 ℃, the vacuum degree is 40Pa, and the rotating speed of the screw is 105rp, and finally obtaining the polysiloxane with ultrahigh viscosity and ultralow volatility.
Example 6:
1) continuously adding hydrogen siloxane, polyether or olefin and platinum complex solution of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane into a first series of continuous stirred tank reactors for mixing, wherein the stirring speed is 150rpm, the feeding amount of the hydrogen siloxane is 100kg/h, the feeding amount of the polyether or olefin is 0.3kg/h, the feeding amount of the platinum complex solution of the chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane is 0.03kg/h, and the mixing temperature is 170 ℃;
2) discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last series of continuous stirred tank reactors;
3) the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300rpm for 2 h;
4) adding silazane in a feeding amount of 0.03kg/h to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
5) discharging the polysiloxane mixed product into a falling strip devolatilizer for pre-devolatilization; the pre-devolatilization temperature is 160 ℃, and the vacuum degree is 70 Pa;
6) and finally, carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain polysiloxane, wherein the temperature of a screw barrel is 200 ℃, the vacuum degree is 40Pa, and the rotating speed of the screw is 105rp, and finally obtaining the polysiloxane with ultrahigh viscosity and ultralow volatility.
Table 1: the viscosity behavior of the compositions of examples 1-6 is shown after t 0 days after production and after 30 days of storage.
TABLE 1
As can be seen from all the examples described above, low-viscosity, storage-stable organopolysiloxane compositions were prepared between the continuously produced polysiloxanes of the invention by setting the feed rate of the hydrogensiloxanes and also the temperature and vacuum of the preliminary devolatilization.
The embodiments of the present invention are the preferred embodiments of the present invention, and the scope of the present invention is not limited by the embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (5)
1. A method for the continuous production of polysiloxanes, comprising the steps of:
step 1: continuously adding hydrosiloxane, polyether or olefin and catalyst solution into at least one series of continuous stirred tank reactors to mix;
step 2: discharging a mixture containing the siloxane copolymer and unreacted hydrogen siloxane and olefin or polyether from the outlet of the last continuous stirred tank reactor;
and step 3: the mixture was fed on to a continuous mixer and subjected to shear generated by 2 dissolver discs at 1300 rpm;
and 4, step 4: adding a terminator to terminate the reaction in the continuous mixer to obtain a polysiloxane mixed product;
and 5: pre-devolatilizing the polysiloxane mixed product in a falling strip devolatilizer;
step 6: and carrying out secondary enhanced devolatilization on the pre-devolatilized polysiloxane mixed product in a double-screw extruder to obtain the polysiloxane.
2. The continuous production method according to claim 1, wherein in step 1, the catalyst is a platinum complex of chloroplatinic acid and 1, 3-divinyltetramethyldisiloxane.
3. The continuous production method according to claim 1, wherein the mixing temperature in step 1 is 170 to 190 ℃.
4. The continuous production method according to claim 1, wherein in step 4, the terminating agent is one selected from diethylamine, tri-n-butylamine, trinonyl amine, and silazane.
5. The continuous production method according to claim 1, wherein in the step 5, the temperature of the pre-devolatilization is 140 to 160 ℃, and the vacuum degree of the pre-devolatilization is 60 to 100 Pa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115212824A (en) * | 2022-08-23 | 2022-10-21 | 合盛硅业股份有限公司 | System for be used for producing high viscosity 107 glue |
| WO2024051671A1 (en) * | 2022-09-06 | 2024-03-14 | 江西蓝星星火有机硅有限公司 | Polymerization-termination device and method for continuous production of organopolysiloxanes |
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| CN115212824B (en) * | 2022-08-23 | 2023-08-29 | 合盛硅业(嘉兴)有限公司 | System for be used for producing high viscosity 107 glue |
| WO2024051671A1 (en) * | 2022-09-06 | 2024-03-14 | 江西蓝星星火有机硅有限公司 | Polymerization-termination device and method for continuous production of organopolysiloxanes |
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