CN115317941B - Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification - Google Patents
Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification Download PDFInfo
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- CN115317941B CN115317941B CN202211019283.5A CN202211019283A CN115317941B CN 115317941 B CN115317941 B CN 115317941B CN 202211019283 A CN202211019283 A CN 202211019283A CN 115317941 B CN115317941 B CN 115317941B
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 141
- WOXXJEVNDJOOLV-UHFFFAOYSA-N ethenyl-tris(2-methoxyethoxy)silane Chemical compound COCCO[Si](OCCOC)(OCCOC)C=C WOXXJEVNDJOOLV-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 128
- 239000002994 raw material Substances 0.000 claims abstract description 68
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 34
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 238000010992 reflux Methods 0.000 claims description 13
- 238000005086 pumping Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 229910052593 corundum Inorganic materials 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 2
- 229920004933 Terylene® Polymers 0.000 claims description 2
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims description 2
- 229910001701 hydrotalcite Inorganic materials 0.000 claims description 2
- 229960001545 hydrotalcite Drugs 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000011874 heated mixture Substances 0.000 claims 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims 1
- -1 beta-methoxyethoxy Chemical group 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 5
- 238000005809 transesterification reaction Methods 0.000 abstract description 5
- 239000003513 alkali Substances 0.000 abstract description 4
- 238000005260 corrosion Methods 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000011282 treatment Methods 0.000 abstract 1
- 238000004821 distillation Methods 0.000 description 10
- 239000002585 base Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 7
- 238000012856 packing Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 238000006136 alcoholysis reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical group [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000015320 potassium carbonate Nutrition 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- GQIUQDDJKHLHTB-UHFFFAOYSA-N trichloro(ethenyl)silane Chemical compound Cl[Si](Cl)(Cl)C=C GQIUQDDJKHLHTB-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000005050 vinyl trichlorosilane Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- 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
- C07F7/18—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
-
- 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
- C07F7/18—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
- C07F7/188—Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification. Belongs to the technical field of catalytic rectification, and comprises the following specific steps: raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane enter from the middle part of a catalytic rectifying tower, and under the catalytic action of solid alkali, the two raw materials undergo transesterification reaction in a reaction section and undergo gas-liquid mass transfer, so that a continuous catalytic rectifying process is realized. The invention adopts solid alkali as catalyst and catalytic rectification technology, can continuously operate, simplifies the process flow, improves the product yield, avoids the corrosion of the traditional liquid alkali to reaction equipment, and has the characteristics of low energy consumption, low material consumption, high reaction conversion rate, high product purity and the like. The invention integrates catalytic reaction and rectification into a whole to obtain the target product vinyltris (beta-methoxyethoxy) silane, and the subsequent treatments such as separation are not needed, so that the yield of the final product vinyltris (beta-methoxyethoxy) silane is 80%, and the purity can reach more than 99%.
Description
Technical Field
The invention belongs to the technical field of catalytic distillation, and relates to a method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic distillation; in particular to a method for preparing vinyl tri (beta-methoxyethoxy) silane by using a catalytic rectification reaction device.
Background
In the prior art, vinyl tri (beta-methoxyethoxy) silane is a novel organosilicon compound, has been paid attention to in the field of novel safety electrolyte of lithium ion batteries, can be used as a coupling agent with excellent performance, an excellent release agent in the rubber and plastic processing industry, an additive in the production of daily cosmetics and the like, and has very wide application.
The synthesis method of vinyl tri (beta-methoxyethoxy) silane is mainly divided into two types: alcoholysis and transesterification processes.
The alcoholysis method is to synthesize vinyl tri (beta-methoxyethoxy) silane by using vinyl trichlorosilane and ethylene glycol monomethyl ether as raw materials and performing alcoholysis reaction. The byproduct obtained by the method is hydrogen chloride gas, which is easy to corrode equipment. The transesterification method is to take vinyl trimethoxy silane and ethylene glycol monomethyl ether as raw materials, naOH as a catalyst to perform transesterification reaction to synthesize vinyl tri (beta-methoxyethoxy) silane, the catalyst is not easy to separate after the reaction is finished, the reaction solution is alkaline, and the purity of the target product is not high.
Disclosure of Invention
The invention aims to: the invention aims to provide a method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification, which has the advantages of simple and convenient process, environmental protection and no pollution, and the prepared product has higher purity.
The technical scheme of the invention is as follows: the invention discloses a catalytic rectification reaction device, which comprises an ethylene glycol monomethyl ether raw material tank, a vinyl trimethoxy silane raw material tank, a raw material mixer, a catalytic rectification tower, a condenser, a reboiler, a methanol product tank, a pump, a product rectification tower, an unreacted complete raw material tank and a vinyl tri (beta-methoxyethoxy) silane product tank;
the catalytic rectifying tower comprises a catalytic rectifying tower top at the upper end, a catalytic rectifying tower rectifying section at the lower side of the catalytic rectifying tower top, a catalytic rectifying tower middle part at the middle end, a catalytic rectifying tower reaction section at the lower end and a catalytic rectifying tower kettle at the bottom side of the catalytic rectifying tower reaction section;
the product rectifying tower comprises a product rectifying tower top at the upper end, a product rectifying tower rectifying section at the lower side of the product rectifying tower top, a product rectifying tower stripping section at the middle end and a product rectifying tower kettle at the bottom side of the product rectifying tower stripping section at the lower end;
Connecting pipelines are respectively arranged at one end of the ethylene glycol monomethyl ether raw material tank and one end of the vinyl trimethoxy silane raw material tank, the other ends of the two connecting pipelines are respectively summarized into a main pipeline after passing through a first arranged pump, the main pipeline is connected to a raw material mixer, and the other end of the raw material mixer is connected to the middle part of a catalytic rectifying tower of the catalytic rectifying tower through the arranged connecting pipelines;
one end of the top of the catalytic rectifying tower is connected to a first condenser through a connecting pipeline, two connecting pipelines are arranged at the other end of the first condenser, one connecting pipeline is connected to the other end of the top of the catalytic rectifying tower, and the other connecting pipeline is connected to a methanol product tank;
The catalytic rectifying tower kettle is connected to one side of a first reboiler through a connecting pipeline, and two connecting pipelines are respectively arranged at the other two ends of the reboiler;
One connecting pipeline is connected to the other end of the tower kettle of the catalytic rectifying tower, the other connecting pipeline is connected to a second pump, and the other end of the pump is connected to the middle part of the product rectifying tower through the connecting pipeline;
One end of the top of the product rectifying tower is connected to the second condenser through a connecting pipeline, two connecting pipelines are arranged at the other end of the second condenser, one connecting pipeline is connected to the other connecting end of the top of the product rectifying tower, the other connecting pipeline is connected to an unreacted complete raw material tank,
The product rectifying tower kettle is connected to one side of a second reboiler through a connecting pipeline, and two connecting pipelines are respectively arranged at the other two ends of the reboiler;
one connecting pipeline is connected to the other end of the tower kettle of the product rectifying tower, and the other connecting pipeline is connected to a vinyl tri (beta-methoxyethoxy) silane product tank;
the catalytic rectifying tower is a packed tower, the height of the packed tower is 2.5m, wherein the height of a rectifying section of the catalytic rectifying tower is 1m, and the height of a reaction section of the catalytic rectifying tower is 1m; the rest is the heights of the top of the catalytic rectifying tower, the middle part of the catalytic rectifying tower and the bottom of the catalytic rectifying tower;
the product rectifying tower is a packed tower, the height of the packed tower is 3.5m, wherein the height of a rectifying section of the product rectifying tower is 1.4m, and the height of a stripping section of the product rectifying tower is 1.6m; the rest is the heights of the top of the product rectifying tower, the middle part of the product rectifying tower and the bottom of the product rectifying tower;
the preparation method comprises the following steps:
Firstly, raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are respectively conveyed into a pump through an ethylene glycol monomethyl ether raw material tank and a vinyl trimethoxy silane raw material tank, then conveyed into a raw material mixer through the pump for mixing, and conveyed into a catalytic rectifying tower through a connecting pipeline for catalytic rectifying reaction after being mixed, so that by-product methanol, product vinyl tri (beta-methoxyethoxy) silane and unreacted raw materials are generated;
secondly, after reaction, evaporating methanol steam from the top of the catalytic rectifying tower, sending the methanol steam to a first condenser for condensation through a connecting pipeline at the top of the catalytic rectifying tower, wherein part of the methanol steam flows back into the top of the catalytic rectifying tower, and the other part of the methanol steam finally enters a methanol product tank through the connecting pipeline;
the mixed solution of unreacted raw materials and vinyl tri (beta-methoxyethoxy) silane is taken out from the tower bottom of the catalytic rectifying tower and is sent to a first reboiler for heating through a connecting pipeline,
After being heated by a reboiler, one part of the liquid returns to the bottom of the catalytic rectifying tower, and the other part of the liquid enters a second pump through a connecting pipeline;
Finally, pumping the mixed solution of unreacted complete raw material and vinyl tri (beta-methoxyethoxy) silane entering the second pump into a product rectifying tower through a connecting pipeline for separation, evaporating unreacted complete raw material steam from the top of the product rectifying tower, conveying the unreacted complete raw material steam into a second condenser through the connecting pipeline for condensation through the top of the product rectifying tower, and after condensation, refluxing one part of the unreacted complete raw material steam into the top of the product rectifying tower, and conveying the other part of the unreacted complete raw material steam into an unreacted complete raw material tank through the connecting pipeline;
taking out the product vinyl tri (beta-methoxyethoxy) silane from the tower bottom of the product rectifying tower, heating the product vinyl tri (beta-methoxyethoxy) silane by a second reboiler, refluxing one part of the product vinyl tri (beta-methoxyethoxy) silane into the tower bottom of the product rectifying tower, and conveying the other part of the product vinyl tri (beta-methoxyethoxy) silane to a product tank through a connecting pipeline;
the feeding mole ratio of the vinyl trimethoxy silane to the ethylene glycol monomethyl ether is 1: 2-1: 4, a step of;
The pressure of the catalytic rectifying tower is 0.8-1 MPa, and the reflux ratio of the catalytic rectifying tower is 1-5;
the temperature of the top of the catalytic rectifying tower is 55-65 ℃;
the temperature of the tower bottom of the catalytic rectifying tower is 120-140 ℃;
the temperature of the reaction section of the catalytic rectifying tower is 90-120 ℃;
a solid base catalyst is filled in the reaction section of the catalytic rectifying tower, and the filled solid base catalyst is one of K2CO 3/gamma Al2O3, KF/CaO, KF/gamma Al2O3, ca-Al hydrotalcite, KOH/gamma Al2O3 and KF/MgO-CeO 2;
The filled solid base catalyst is arranged in a nylon cloth or terylene cloth small bag and then is fixed by a stainless steel wire mesh corrugated filler;
the catalytic rectifying tower is a packed tower, and the packing is stainless steel wire mesh corrugated packing, wherein only the packing is arranged in a rectifying section of the catalytic rectifying tower, and a catalyst is fixed in the packing in a reaction section of the catalytic rectifying tower;
The operating pressure of the product rectifying tower is 0.18-0.2 MPa, and the reflux ratio of the product rectifying tower is 2-4;
The temperature of the top of the product rectifying tower is 70-80 ℃, and the temperature of the bottom of the product rectifying tower is 210-220 ℃;
the product rectifying tower is a packed tower, and packing stainless steel wire mesh corrugated packing is arranged in both the rectifying section and the stripping section of the product rectifying tower.
The beneficial effects of the invention are as follows: the method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic distillation integrates reaction and separation, the separation process and the reaction process are mutually promoted, the yield and the yield of products are effectively improved, and meanwhile, the heat of reaction is fully utilized, so that the energy consumption of distillation is reduced; continuous catalytic rectification can realize large-scale continuous production, and the product quality is stable; the continuous catalytic rectification adopts solid alkali as a catalyst, has small corrosion to equipment, is environment-friendly, is easier to separate from liquid products, has higher activity and selectivity, and has longer catalytic life; meanwhile, the serious corrosion phenomenon of equipment is relieved, the catalyst adopts a filling technology, the separation difficulty is reduced, the catalyst can be recycled, the cost is reduced, the resources are saved, and good economic benefit is created; compared with the prior art, the method has the characteristics of simple process, easy operation, low hazard, high safety, reasonable device structure, low equipment investment, low energy consumption, high conversion rate, high product purity and the like. The invention has the advantages of reaching the indexes.
Drawings
FIG. 1 is a schematic diagram of a catalytic rectification reaction apparatus in accordance with the present invention;
Wherein 1 is a ethylene glycol monomethyl ether raw material tank, 2 is a vinyl trimethoxy silane raw material tank, 3 is a raw material mixer, 4 is a condenser, 5 is a catalytic rectifying tower rectifying section, 6 is a catalytic rectifying tower reaction section, 7 is a reboiler, 8 is a methanol product tank, 9 is a pump, 10 is a product rectifying tower rectifying section, 11 is a product rectifying tower stripping section, 12 is an unreacted complete raw material tank, and 13 is a vinyl tri (beta-methoxyethoxy) silane product tank.
Detailed Description
The invention is described in further detail below in connection with the examples, it being noted that the scope of the invention is not limited to the following examples, which are presented for illustrative purposes only and are not intended to limit the invention in any way.
As shown in the figure, the catalytic reaction rectifying tower sequentially comprises a catalytic rectifying tower top, a catalytic rectifying tower rectifying section 5, a catalytic rectifying tower middle part, a catalytic rectifying tower reaction section 6 and a catalytic rectifying tower kettle from top to bottom;
Wherein, the material of catalytic distillation tower rectifying section 5 and catalytic distillation tower reaction section 6 two parts is stainless steel 304, and its internal diameter is 260mm, and the filler is wire net ripple filler, catalytic distillation tower's height is 2m, and theoretical plate number is about 10, and wherein, catalytic distillation tower rectifying section 5's height is 1m, and theoretical plate number is about 5, catalytic distillation tower reaction section 6 height 1m, and solid base catalyst is K2CO3/Al2O3 in the catalytic distillation tower reaction section 6, and the filler is wire net ripple (500, BX), solid base catalyst and wire net ripple filler with 1:2, uniformly distributing the catalyst on the surface of the corrugated filler of the metal wire mesh, fixing, and then loading into a reaction section 6 (5 th to 10 th theoretical plates from top to bottom) of the catalytic rectifying tower.
The product rectifying tower is a packed tower, the packing is the same as that of the catalytic rectifying tower, and the tower body sequentially comprises a product rectifying tower top, a product rectifying tower rectifying section 10, a product rectifying tower middle part, a product rectifying tower stripping section 11 and a product rectifying tower kettle from top to bottom;
the product rectifying tower rectifying section 10 and the product rectifying tower stripping section 11 are made of stainless steel 304, the inner diameter is 220mm, the height of the product rectifying tower is 3.5m, the height of the product rectifying tower rectifying section 10 is 1.4m, and the height of the product rectifying tower stripping section 11 is 1.6m; the theoretical plate number of the rectifying section 10 of the product rectifying tower is about 7, and the theoretical plate number of the stripping section 11 of the product rectifying tower is about 8.
The gas chromatographic analysis of the product is as follows: SE-54 (30 m x 0.32mm x 0.50 um) capillary chromatography column, FID hydrogen flame detector; the initial temperature is 130 ℃, the final temperature is 280 ℃, the initial temperature is 8min, and the heating rate is 15 ℃ and min-1; the temperature of the detector is 300 ℃, the temperature of the vaporization chamber is 300 ℃, the flow rate of carrier gas is 40mL min < -1 >, the sample injection amount is 0.1uL, and the separation ratio is 1/30;
The method for preparing the vinyl tri (beta-methoxyethoxy) silane by using the catalytic rectification reaction device comprises the following specific steps:
Raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are respectively conveyed into a pump 9 through an ethylene glycol monomethyl ether raw material tank 1 and a vinyl trimethoxy silane raw material tank 2, then conveyed into a raw material mixer 9 through the pump 9 for mixing, conveyed into the middle part of a catalytic rectifying tower through a connecting pipeline after being mixed, then enter the catalytic rectifying tower from the middle part of the catalytic rectifying tower through the pump, and the ethylene glycol monomethyl ether and the vinyl trimethoxy silane perform countercurrent heat and mass transfer in a reaction section of the catalytic rectifying tower, and perform transesterification reaction under the action of a solid base catalyst in a reaction section 6 of the catalytic rectifying tower; after the ethylene glycol monomethyl ether and the vinyl trimethoxy silane react, the top of the tower is high-purity methanol, and the bottom of the tower is mixed liquid of unreacted raw materials and vinyl tri (beta-methoxyethoxy) silane; and separating unreacted raw materials and the vinyl tri (beta-methoxyethoxy) silane mixed solution by a product rectifying tower, and then obtaining the vinyl tri (beta-methoxyethoxy) silane with higher purity from the tower bottom.
Example 1
Adopting the technological process shown in figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are prepared by the following steps: 1, feeding at normal temperature, wherein the flow rate of ethylene glycol monomethyl ether is 91.3kg/h, the flow rate of vinyl trimethoxy silane is 59.3kg/h, respectively, feeding the ethylene glycol monomethyl ether into a 5 th plate of a rectifying section 5 of a catalytic rectifying tower from respective raw material storage tanks through a pump 9, wherein the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 97 ℃, the temperature at the top of the catalytic rectifying tower is stabilized at 58.7 ℃, the temperature at the bottom of the catalytic rectifying tower is stabilized at 135.8 ℃, the reflux ratio at the top of the catalytic rectifying tower is controlled at 4:1, and then pumping unreacted raw materials and products at the bottom of the catalytic rectifying tower into a product rectifying tower for separation; the yield of the catalytic rectifying tower product was found to be 60% by gas phase analysis, and the purity of the rectifying tower product vinyltris (beta-methoxyethoxy) silane was found to be 99.2%.
Example 2
The process flow shown in the attached figure 1 is adopted, and the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are prepared according to the following ratio of 3.5:1, feeding at normal temperature, wherein the flow of ethylene glycol monomethyl ether is 106.5kg/h, the flow of vinyl trimethoxy silane is 59.3kg/h, respectively, feeding the ethylene glycol monomethyl ether into a5 th plate of a rectifying section 5 of a catalytic rectifying tower from respective raw material storage tanks through a pump 9, wherein the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 99 ℃, the temperature at the top of the catalytic rectifying tower is stabilized at 62 ℃, the temperature at the bottom of the catalytic rectifying tower is stabilized at 135.7 ℃, the reflux ratio is controlled to be 4:1, and then pumping unreacted raw materials and products in the bottom of the catalytic rectifying tower into a product rectifying tower for separation; the yield of the catalytic rectifying tower product was found to be 78% by gas phase analysis, and the purity of the rectifying tower product vinyltris (beta-methoxyethoxy) silane was found to be 99.5%.
Example 3
Adopting the technological process shown in figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are prepared by the following steps: 1, feeding at normal temperature, wherein the flow of ethylene glycol monomethyl ether is 121.7kg/h, the flow of vinyl trimethoxy silane is 59.3kg/h, respectively, pumping the ethylene glycol monomethyl ether into a 5 th plate of a rectifying section of a catalytic rectifying tower from respective raw material storage tanks, wherein the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 100 ℃, the temperature at the top of the catalytic rectifying tower is 65 ℃, the temperature at the bottom of the catalytic rectifying tower is 135.5 ℃, the reflux ratio is controlled to be 4:1, and then pumping unreacted raw materials and products in the bottom of the catalytic rectifying tower into a product rectifying tower for separation; after the reaction, the yield of the catalytic rectifying tower product is 80%, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is 99.8% through gas phase analysis.
Comparative example 1
Adopting the technological process shown in figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are prepared by the following steps: 1, feeding at normal temperature, wherein the flow of ethylene glycol monomethyl ether is 121.7kg/h, the flow of vinyl trimethoxy silane is 59.3kg/h, respectively, pumping the ethylene glycol monomethyl ether into a5 th plate of a rectifying section of a catalytic rectifying tower from respective raw material storage tanks, wherein the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 100 ℃, the temperature at the top of the catalytic rectifying tower is 65 ℃, the temperature at the bottom of the catalytic rectifying tower is 135.5 ℃, the reflux ratio is controlled to be 0, and then pumping unreacted raw materials and products in the bottom of the catalytic rectifying tower into a product rectifying tower for separation; after the reaction, the yield of the catalytic rectifying tower product is found to be 50% by gas phase analysis, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is found to be 90%.
Comparative example 2
Adopting the technological process shown in figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are prepared by the following steps: 1, wherein the molar ratio is that the ethylene glycol monomethyl ether is fed at normal temperature, the flow of ethylene glycol monomethyl ether is 121.7kg/h, the flow of vinyl trimethoxy silane is 59.3kg/h, the ethylene glycol monomethyl ether is pumped into a 5 th plate of a rectifying section of a catalytic rectifying tower from respective raw material storage tanks, compared with the method in which the solid base catalyst is not filled in a reaction section 6 of the catalytic rectifying tower in the embodiment of 1-3, the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 100 ℃, the temperature at the top of the catalytic rectifying tower is stabilized at 65 ℃, the temperature at the bottom of the catalytic rectifying tower is stabilized at 135.5 ℃, the reflux ratio is controlled to be 4:1, and unreacted raw materials and products in the bottom of the catalytic rectifying tower are pumped into a product rectifying tower for separation; after the reaction, the yield of the catalytic rectifying tower product is found to be 45% by gas phase analysis, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is found to be 87%.
Finally, it should be understood that the embodiments described herein are merely illustrative of the principles of the embodiments of the present invention; other variations are possible within the scope of the invention; accordingly, the embodiments of the present invention are not limited to the embodiments explicitly described and depicted herein.
Claims (1)
1. A method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification is characterized in that: the catalytic rectification reaction device comprises an ethylene glycol monomethyl ether raw material tank (1), a vinyl trimethoxy silane raw material tank (2), a raw material mixer (3), a catalytic rectification tower, a condenser (4), a reboiler (7), a methanol product tank (8), a pump (9), a product rectification tower, an unreacted complete raw material tank (12) and a vinyl tri (beta-methoxyethoxy) silane product tank (13);
The catalytic rectifying tower comprises a catalytic rectifying tower top at the upper end, a catalytic rectifying tower rectifying section (5) at the lower side of the catalytic rectifying tower top, a catalytic rectifying tower reaction section (6) at the middle and lower ends of the catalytic rectifying tower and a catalytic rectifying tower kettle at the bottom side of the catalytic rectifying tower reaction section (6);
the product rectifying tower comprises a product rectifying tower top at the upper end, a product rectifying tower rectifying section (10) at the lower side of the product rectifying tower top, a product rectifying tower stripping section (11) at the middle end and a product rectifying tower stripping section (11) at the lower end of the product rectifying tower and a product rectifying tower kettle at the bottom side of the product rectifying tower stripping section (11);
Connecting pipelines are respectively arranged at one end of the ethylene glycol monomethyl ether raw material tank (1) and one end of the vinyl trimethoxy silane raw material tank (2), the other ends of the two connecting pipelines are respectively summarized into a main pipeline after passing through a first arranged pump (9) and are connected to a raw material mixer (3), and the other end of the raw material mixer (3) is connected to the middle part of a catalytic rectifying tower of the catalytic rectifying tower through the arranged connecting pipelines;
One end of the top of the catalytic rectifying tower is connected to a first condenser (4) through a connecting pipeline, two connecting pipelines are arranged at the other end of the first condenser (4), one connecting pipeline is connected to the other end of the top of the catalytic rectifying tower, and the other connecting pipeline is connected to a methanol product tank (8);
The bottom of the catalytic rectifying tower is connected to one side of a first reboiler (7) through a connecting pipeline, and two connecting pipelines are respectively arranged at the other two ends of the reboiler (7);
One connecting pipeline is connected to the other end of the tower kettle of the catalytic rectifying tower, the other connecting pipeline is connected to a second pump (9), and the other end of the pump (9) is connected to the middle part of the product rectifying tower through the connecting pipeline;
One end of the top of the product rectifying tower is connected to a second condenser (4) through a connecting pipeline, two connecting pipelines are arranged at the other end of the second condenser (4), one connecting pipeline is connected to the other connecting end of the top of the product rectifying tower, the other connecting pipeline is connected to an unreacted complete raw material tank (12),
The product rectifying tower kettle is connected to one side of a second reboiler (7) through a connecting pipeline, and two connecting pipelines are respectively arranged at the other two ends of the reboiler (7);
one connecting pipeline is connected to the other end of the tower kettle of the product rectifying tower, and the other connecting pipeline is connected to a vinyl tri (beta-methoxyethoxy) silane product tank (13);
the catalytic rectifying tower is a packed tower, the height of the packed tower is 2.5m, the height of the rectifying section (5) of the catalytic rectifying tower is 1m, and the height of the reaction section (6) of the catalytic rectifying tower is 1m;
the product rectifying tower is a packed tower, the height of the packed tower is 3.5m, the height of a rectifying section (10) of the product rectifying tower is 1.4m, and the height of a stripping section (11) of the product rectifying tower is 1.6m;
The preparation method comprises the following steps:
Firstly, raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are respectively conveyed into a pump (9) through an ethylene glycol monomethyl ether raw material tank (1) and a vinyl trimethoxy silane raw material tank (2), then conveyed into a raw material mixer (3) through the pump (9) for mixing, and conveyed into a catalytic rectifying tower through a connecting pipeline for catalytic rectifying reaction after being mixed, so that by-product methanol, product vinyl tri (beta-methoxyethoxy) silane and unreacted complete raw materials are generated;
Secondly, after reaction, evaporating methanol steam from the top of the catalytic rectifying tower, sending the methanol steam to a first condenser (4) through a connecting pipeline at the top of the catalytic rectifying tower for condensation, wherein part of the methanol steam flows back into the top of the catalytic rectifying tower, and the other part of the methanol steam finally enters a methanol product tank (8) through the connecting pipeline;
The mixed solution of unreacted raw materials and vinyl tri (beta-methoxyethoxy) silane is taken out from the tower bottom of the catalytic rectifying tower and is sent to a first reboiler (7) for heating through a connecting pipeline,
After being heated by a reboiler (7), one part of the heated mixture returns to the bottom of the catalytic rectifying tower, and the other part of the heated mixture enters a second pump (9) through a connecting pipeline;
finally, pumping the mixed solution of unreacted complete raw material and vinyl tri (beta-methoxyethoxy) silane entering the second pump (9) into a product rectifying tower through a connecting pipeline for separation, evaporating unreacted complete raw material steam from the top of the product rectifying tower, conveying the steam to the second condenser (4) through the connecting pipeline for condensation through the top of the product rectifying tower, and after condensation, refluxing one part of the condensed mixed solution into the top of the product rectifying tower, and feeding the other part of condensed mixed solution into an unreacted complete raw material tank (12) through the connecting pipeline;
Taking out the vinyl tri (beta-methoxyethoxy) silane product from the tower bottom of the product rectifying tower, heating the vinyl tri (beta-methoxyethoxy) silane product by a second reboiler (7), refluxing one part of the vinyl tri (beta-methoxyethoxy) silane product into the tower bottom of the product rectifying tower, and conveying the other part of the vinyl tri (beta-methoxyethoxy) silane product to a vinyl tri (beta-methoxyethoxy) silane product tank (13) through a connecting pipeline;
wherein, the feeding mole ratio of the vinyl trimethoxy silane to the ethylene glycol monomethyl ether is 1: 2-1: 4, a step of;
The pressure of the catalytic rectifying tower is 0.8-1 MPa, and the reflux ratio of the catalytic rectifying tower is 1-5;
the temperature of the top of the catalytic rectifying tower is 55-65 ℃;
the temperature of the tower bottom of the catalytic rectifying tower is 120-140 ℃;
the temperature of the reaction section (6) of the catalytic rectifying tower is 90-120 ℃;
A solid base catalyst is filled in the catalytic rectifying tower reaction section (6), and the filled solid base catalyst is one of K2CO 3/gamma Al2O3, KF/CaO, KF/gamma Al2O3, ca-Al hydrotalcite, KOH/gamma Al2O3 and KF/MgO-CeO 2;
The filled solid base catalyst is arranged in a nylon cloth or terylene cloth small bag and then is fixed by a stainless steel wire mesh corrugated filler;
The operating pressure of the product rectifying tower is 0.18-0.2 MPa, and the reflux ratio of the product rectifying tower is 2-4;
the temperature of the top of the product rectifying tower is 70-80 ℃, and the temperature of the bottom of the product rectifying tower is 210-220 ℃.
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| CN106349276A (en) * | 2016-08-12 | 2017-01-25 | 荆州市江汉精细化工有限公司 | Ester exchange method for preparing vinyl tri-(2- methoxy ethyoxyl)-silane |
| CN109956849A (en) * | 2017-12-22 | 2019-07-02 | 湖南中创化工股份有限公司 | A kind of method preparing ethylene acetate and sec-butyl alcohol and catalyst system and device |
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| CN103708471B (en) * | 2013-12-18 | 2015-09-09 | 天津大学 | Silane through reverse disproportionation prepares the Apparatus and method for of chlorosilane |
| CN103848730B (en) * | 2014-01-09 | 2015-06-17 | 东营市润成碳材料科技有限公司 | Production device system and production process for polymethoxy dimethyl ether (PODE) |
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| CN109956849A (en) * | 2017-12-22 | 2019-07-02 | 湖南中创化工股份有限公司 | A kind of method preparing ethylene acetate and sec-butyl alcohol and catalyst system and device |
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