CN113121585A - Micro-reaction system and method for continuously preparing gamma-chloropropyltrichlorosilane - Google Patents
Micro-reaction system and method for continuously preparing gamma-chloropropyltrichlorosilane Download PDFInfo
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- CN113121585A CN113121585A CN202110430595.4A CN202110430595A CN113121585A CN 113121585 A CN113121585 A CN 113121585A CN 202110430595 A CN202110430595 A CN 202110430595A CN 113121585 A CN113121585 A CN 113121585A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 49
- OOXSLJBUMMHDKW-UHFFFAOYSA-N trichloro(3-chloropropyl)silane Chemical compound ClCCC[Si](Cl)(Cl)Cl OOXSLJBUMMHDKW-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000003860 storage Methods 0.000 claims abstract description 24
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 claims abstract description 17
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 17
- 238000010791 quenching Methods 0.000 claims abstract description 15
- 230000000171 quenching effect Effects 0.000 claims abstract description 15
- 239000003054 catalyst Substances 0.000 claims abstract description 11
- 238000004821 distillation Methods 0.000 claims abstract description 10
- 230000035484 reaction time Effects 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 4
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 24
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 12
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 12
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 12
- 238000007599 discharging Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 239000012190 activator Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000047 product Substances 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000007822 coupling agent Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 229920000459 Nitrile rubber Polymers 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000000565 sealant Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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 Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- 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 Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/20—Purification, separation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a micro-reaction system and a method for continuously preparing gamma-chloropropyltrichlorosilane, wherein the system comprises a chloropropene storage tank, a catalyst storage tank and a trichlorosilane storage tank, wherein the chloropropene storage tank and the catalyst storage tank are connected to a premixing tank through pipelines, a discharge port of the premixing tank is connected with a first discharge pipeline, a discharge port of the trichlorosilane storage tank is connected with a second discharge pipeline, the first discharge pipeline and the second discharge pipeline are connected to a micro mixer, a discharge port of the micro mixer is connected to a micro reactor, the micro reactor is connected with a quenching heat exchanger, a cooling coil is arranged in the quenching heat exchanger, and the quenching heat exchanger is connected with a distillation still. The method preheats materials and then carries out reaction in the microreactor, and the system and the method have the advantages of short reaction time, high efficiency, low reaction by-product and high product purity, and can be widely applied to the field of preparation of gamma-chloropropyltrichlorosilane.
Description
Technical Field
The invention relates to the technical field of production and processing of gamma-chloropropyltrichlorosilane, in particular to a micro-reaction system and a micro-reaction method for continuously preparing gamma-chloropropyltrichlorosilane.
Background
The silane coupling agent is a fourth major organic silicon product following three major products of organic silicon, namely silicone oil, silicone rubber and silicone resin, the position of the silane coupling agent in the organic silicon industry is increasingly important, and the silane coupling agent becomes an indispensable matched chemical auxiliary agent in the modern organic silicon industry, the organic polymer industry, the composite material industry and related high and new technical fields. The glass fiber reinforced plastic composite material is mainly applied to glass fiber reinforced materials and rubber products, and can strengthen the physical properties of the composite material, such as strength, toughness, electrical properties, water resistance, corrosion resistance and the like; in addition, they are also used as adhesives such as epoxy and nitrile rubber, and as tackifiers in sealants such as polyurethane and chloroprene rubber. Wherein, the gamma-chloropropyltrichlorosilane is the most basic monomer in the silane coupling agent, and is the coupling agent monomer which is developed earliest and applied most widely in the coupling agent.
At present, the main production method of gamma-chloropropyltrichlorosilane is the traditional kettle type intermittent addition reaction, and the method has the problems of complex control of the reaction process, long reaction period, high energy consumption, unstable reaction process, high byproduct, low product yield and the like. Therefore, it is necessary to develop a method for preparing gamma-chloropropyltrichlorosilane with high reaction speed, low energy consumption and low byproduct content, so as to improve the production efficiency of gamma-chloropropyltrichlorosilane and reduce the production cost.
Disclosure of Invention
The invention aims to provide a micro-reaction system and a micro-reaction method for continuously preparing gamma-chloropropyltrichlorosilane, which solve the problems of long reaction time, high energy consumption and high byproducts in the process of processing gamma-chloropropyltrichlorosilane by the conventional method.
The technical scheme adopted by the invention for solving the technical problems is as follows: the utility model provides a little reaction system of preparation gamma-chloropropyl trichlorosilane in succession, includes chloropropene storage jar, catalyst storage jar and trichlorosilane storage jar chloropropene storage jar and catalyst storage jar pipe connection to premixing jar, the discharge gate connection of premixing jar is provided with first ejection of compact pipeline, and the discharge gate connection of trichlorosilane storage jar is provided with second ejection of compact pipeline, and first ejection of compact pipeline and second ejection of compact pipeline are connected to the micromixer, and the discharge gate of micromixer is connected to the microreactor, and the microreactor connection is provided with the quenching heat exchanger, is provided with cooling coil in the quenching heat exchanger, the quenching heat exchanger connection is provided with stills.
In order to ensure the temperature required by the reaction, preheaters for preheating the first discharging pipeline and the second discharging pipeline are arranged on the conveying paths of the first discharging pipeline and the second discharging pipeline.
Preferably, the micro mixer is an SL30 type micro mixer, and a constant temperature bath for ensuring the temperature required by the micro reactor is further arranged, and the micro reactor is arranged in the constant temperature bath.
The invention also discloses a micro-reaction method for continuously preparing gamma-chloropropyltrichlorosilane, which comprises the steps of adopting the micro-reaction system, taking trichlorosilane and chloropropene as raw materials, chloroplatinic acid as a main catalyst, m-phenylenediamine as a cocatalyst, triisopropanolamine as an activator and resorcinol as an inhibitor, and reacting in a microreactor; the method specifically comprises the following steps:
1) conveying chloropropene, chloroplatinic acid, m-phenylenediamine, triisopropanolamine and resorcinol together to a premixing tank for mixing, preheating the mixed solution to 50 ℃, and simultaneously preheating trichlorosilane to 50 ℃;
2) the preheated materials are sent into a micro mixer together for mixing, the temperature in the micro mixer is 60-100 ℃,
3) feeding the mixed materials into a reaction product of a reaction in the microreactor, wherein the reaction temperature is 55-135 ℃, the pressure is 0.4-0.9 MPa, and the reaction time is 60-120S;
4) after the reaction is finished, sending the reaction product into a quenching heat exchanger to cool the reaction product to below 40 ℃, and stopping the reaction;
5) and (3) feeding the reaction product into a distillation kettle for distillation, wherein the distillation temperature is 160 ℃, and removing impurities to obtain the gamma-chloropropyltrichlorosilane.
Preferably, the reaction temperature in the step 3) is 90 ℃, the pressure is 0.7MPa, and the reaction time is 60S.
Preferably, the molar ratio of trichlorosilane to chloropropene is 1: 1-1.2, and the weight ratio of chloroplatinic acid to m-phenylenediamine to triisopropanolamine to resorcinol is 1: 1.6-1.8: 2.2-2.5: 3.1 to 3.5.
Preferably, the mass of the chloroplatinic acid, the m-phenylenediamine, the triisopropanolamine and the resorcinol accounts for 0.08-0.015 wt% of the total mass of the reaction raw materials.
The invention has the beneficial effects that: by the reaction system and the method, the reaction time can be greatly shortened, the reaction by-products are low, and the product purity is high. Through practical verification, the purity of the gamma-chloropropyltrichlorosilane can reach 99.7-99.9%, and the yield can reach more than 85%.
The invention will be explained in more detail below with reference to the drawings and examples.
Drawings
FIG. 1 is a schematic diagram of the system of the present invention.
Detailed Description
Example 1: as shown in fig. 1, a micro-reaction system for continuously preparing gamma-chloropropyltrichlorosilane comprises a chloropropene storage tank 1, a catalyst storage tank 2 and a trichlorosilane storage tank 3, wherein the chloropropene storage tank 1 and the catalyst storage tank 2 are connected to a premixing tank 4 through pipelines, premixing is carried out in the premixing tank 4, and a feeding pump and a flow meter are arranged on a conveying pipeline and used for controlling feeding amount. Mix jar 4 discharge gate connection in advance and be provided with first ejection of compact pipeline 5, the discharge gate connection of trichlorosilane storage jar 3 is provided with second ejection of compact pipeline 6, and first ejection of compact pipeline 5 and second ejection of compact pipeline 6 are connected to micromixer 7, and the discharge gate of micromixer 7 is connected to microreactor 8, and microreactor 8 connects and is provided with quenching heat exchanger 10, is provided with cooling coil 9 in the quenching heat exchanger 10, quenching heat exchanger 10 connects and is provided with stills 11. And a preheater 12 for preheating the first discharge pipeline 5 and the second discharge pipeline 6 is arranged on the conveying path of the first discharge pipeline 5 and the second discharge pipeline 6.
The micro mixer 7 is an SL30 type micro mixer, a constant temperature bath 13 for ensuring the temperature required by the micro reactor is also arranged, and the micro reactor 8 is arranged in the constant temperature bath 13.
Example 2:
a micro-reaction method for continuously preparing gamma-chloropropyltrichlorosilane adopts the micro-reaction system described in the embodiment 1, trichlorosilane and chloropropene are used as raw materials, chloroplatinic acid is used as a main catalyst, m-phenylenediamine is used as a cocatalyst, triisopropanolamine is used as an activator, and resorcinol is used as an inhibitor, and the reaction is carried out in a microreactor; the molar ratio of trichlorosilane to chloropropene is 1: 1-1.2, and the weight ratio of chloroplatinic acid, m-phenylenediamine, triisopropanolamine and resorcinol is 1: 1.6-1.8: 2.2-2.5: 3.1 to 3.5. The mass of the chloroplatinic acid, the m-phenylenediamine, the triisopropanolamine and the resorcinol accounts for 0.08-0.015 wt% of the total mass of the reaction raw materials.
The method specifically comprises the following steps:
1) conveying chloropropene, chloroplatinic acid, m-phenylenediamine, triisopropanolamine and resorcinol together to a premixing tank for mixing, preheating the mixed solution to 50 ℃, and simultaneously preheating trichlorosilane to 50 ℃;
2) the preheated materials are sent into a micro mixer together for mixing, the temperature in the micro mixer is 60-100 ℃,
3) feeding the mixed materials into a reaction product of a reaction in the microreactor, wherein the reaction temperature is 55-135 ℃, the pressure is 0.4-0.9 MPa, and the reaction time is 60-120S;
4) after the reaction is finished, sending the reaction product into a quenching heat exchanger to cool the reaction product to below 40 ℃, and stopping the reaction;
5) and (3) feeding the reaction product into a distillation kettle for distillation, wherein the distillation temperature is 160 ℃, and removing impurities to obtain the gamma-chloropropyltrichlorosilane.
Preferably, the reaction temperature in the step 3) is 90 ℃, the pressure is 0.7MPa, and the reaction time is 60S.
The invention is described above with reference to the accompanying drawings. It is to be understood that the specific implementations of the invention are not limited in this respect. Various insubstantial improvements are made by adopting the method conception and the technical scheme of the invention; the present invention is not limited to the above embodiments, and can be modified in various ways.
Claims (7)
1. A micro reaction system for continuously preparing gamma-chloropropyltrichlorosilane is characterized in that: including chloropropene storage jar (1), catalyst storage jar (2) and trichlorosilane storage jar (3), chloropropene storage jar (1) and catalyst storage jar (2) pipe connection are to premixing jar (4), the discharge gate connection of premixing jar (4) is provided with first ejection of compact pipeline (5), the discharge gate connection of trichlorosilane storage jar (3) is provided with second ejection of compact pipeline (6), first ejection of compact pipeline (5) and second ejection of compact pipeline (6) are connected to micro mixer (7), the discharge gate of micro mixer (7) is connected to microreactor (8), microreactor (8) are connected and are provided with quenching heat exchanger (10), be provided with cooling coil (9) in quenching heat exchanger (10), quenching heat exchanger (10) are connected and are provided with stills (11).
2. The micro-reaction system for continuously preparing gamma-chloropropyltrichlorosilane according to claim 1, wherein: and a preheater (12) for preheating the first discharging pipeline (5) and the second discharging pipeline (6) is arranged on the conveying path of the first discharging pipeline (5) and the second discharging pipeline (6).
3. The micro-reaction system for continuously preparing gamma-chloropropyltrichlorosilane according to claim 1, wherein: the micro mixer (7) is an SL30 type micro mixer, a constant temperature bath (13) for ensuring the temperature required by the micro reactor is further arranged, and the micro reactor (8) is arranged in the constant temperature bath (13).
4. A micro-reaction method for continuously preparing gamma-chloropropyltrichlorosilane is characterized by comprising the following steps: the micro-reaction system of claims 1 to 3 is adopted, trichlorosilane and chloropropene are taken as raw materials, chloroplatinic acid is taken as a main catalyst, m-phenylenediamine is taken as a cocatalyst, triisopropanolamine is taken as an activator, and resorcinol is taken as an inhibitor, and the reaction is carried out in a microreactor; the method specifically comprises the following steps:
1) conveying chloropropene, chloroplatinic acid, m-phenylenediamine, triisopropanolamine and resorcinol together to a premixing tank for mixing, preheating the mixed solution to 50 ℃, and simultaneously preheating trichlorosilane to 50 ℃;
2) the preheated materials are sent into a micro mixer together for mixing, the temperature in the micro mixer is 60-100 ℃,
3) feeding the mixed materials into a reaction product of a reaction in the microreactor, wherein the reaction temperature is 55-135 ℃, the pressure is 0.4-0.9 MPa, and the reaction time is 60-120S;
4) after the reaction is finished, sending the reaction product into a quenching heat exchanger to cool the reaction product to below 40 ℃, and stopping the reaction;
5) and (3) feeding the reaction product into a distillation kettle for distillation, wherein the distillation temperature is 160 ℃, and removing impurities to obtain the gamma-chloropropyltrichlorosilane.
5. The micro-reaction process for continuously preparing gamma-chloropropyltrichlorosilane according to claim 1, characterized in that: in the step 3), the reaction temperature is 90 ℃, the pressure is 0.7MPa, and the reaction time is 60S.
6. The micro-reaction process for continuously preparing gamma-chloropropyltrichlorosilane according to claim 1, characterized in that: the molar ratio of trichlorosilane to chloropropene is 1: 1-1.2, and the weight ratio of chloroplatinic acid, m-phenylenediamine, triisopropanolamine and resorcinol is 1: 1.6-1.8: 2.2-2.5: 3.1 to 3.5.
7. The micro-reaction process for continuously preparing gamma-chloropropyltrichlorosilane according to claim 1, characterized in that: the mass of the chloroplatinic acid, the m-phenylenediamine, the triisopropanolamine and the resorcinol accounts for 0.08-0.015 wt% of the total mass of the reaction raw materials.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110430595.4A CN113121585A (en) | 2021-04-21 | 2021-04-21 | Micro-reaction system and method for continuously preparing gamma-chloropropyltrichlorosilane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110430595.4A CN113121585A (en) | 2021-04-21 | 2021-04-21 | Micro-reaction system and method for continuously preparing gamma-chloropropyltrichlorosilane |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457582A (en) * | 2021-07-21 | 2021-10-01 | 江西宏柏新材料股份有限公司 | Device for continuously producing cyanoethyl trichlorosilane |
| CN114292291A (en) * | 2022-01-18 | 2022-04-08 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of gamma-aminopropyl triethoxysilane |
| CN115025731A (en) * | 2022-07-12 | 2022-09-09 | 辽宁石化职业技术学院 | Continuous production device and process of o-phenylphenol |
-
2021
- 2021-04-21 CN CN202110430595.4A patent/CN113121585A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113457582A (en) * | 2021-07-21 | 2021-10-01 | 江西宏柏新材料股份有限公司 | Device for continuously producing cyanoethyl trichlorosilane |
| CN113457582B (en) * | 2021-07-21 | 2022-07-01 | 江西宏柏新材料股份有限公司 | Device for continuously producing cyanoethyl trichlorosilane |
| CN114292291A (en) * | 2022-01-18 | 2022-04-08 | 浙江锦华新材料股份有限公司 | Solvent-free synthesis method of gamma-aminopropyl triethoxysilane |
| CN115025731A (en) * | 2022-07-12 | 2022-09-09 | 辽宁石化职业技术学院 | Continuous production device and process of o-phenylphenol |
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