CN115317941A - Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic distillation - Google Patents
Method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic distillation Download PDFInfo
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- CN115317941A CN115317941A CN202211019283.5A CN202211019283A CN115317941A CN 115317941 A CN115317941 A CN 115317941A CN 202211019283 A CN202211019283 A CN 202211019283A CN 115317941 A CN115317941 A CN 115317941A
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- silane
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- 230000003197 catalytic effect Effects 0.000 title claims abstract description 144
- 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 50
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004821 distillation Methods 0.000 title claims description 48
- 239000000047 product Substances 0.000 claims abstract description 116
- 239000002994 raw material Substances 0.000 claims abstract description 69
- 238000006243 chemical reaction Methods 0.000 claims abstract description 53
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims abstract description 29
- 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 19
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 51
- 238000010992 reflux Methods 0.000 claims description 9
- 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
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims description 4
- 239000006227 byproduct Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000004677 Nylon Substances 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
- 229920000728 polyester Polymers 0.000 claims description 2
- 239000002351 wastewater Substances 0.000 claims 2
- 239000003513 alkali Substances 0.000 abstract description 4
- 239000000463 material 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
- 238000005516 engineering process Methods 0.000 abstract description 2
- 125000004185 ester group Chemical group 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract 1
- 208000012839 conversion disease Diseases 0.000 abstract 1
- 239000012467 final product Substances 0.000 abstract 1
- 238000011282 treatment Methods 0.000 abstract 1
- 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
- 238000005086 pumping Methods 0.000 description 4
- 238000006136 alcoholysis reaction Methods 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 238000005809 transesterification reaction Methods 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical group [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000002912 waste gas 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
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation 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
- 238000004519 manufacturing process Methods 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
- 238000002360 preparation method Methods 0.000 description 1
- 150000003377 silicon compounds Chemical class 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
Images
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
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- 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: ethylene glycol monomethyl ether and vinyl trimethoxy silane as raw materials enter the catalytic rectifying tower from the middle part, and under the catalytic action of solid alkali, the two raw materials undergo an ester exchange reaction and carry out gas-liquid mass transfer in a reaction section, so that a continuous catalytic rectifying process is realized. The method adopts solid alkali as a catalyst and a 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 vinyl tri (beta-methoxyethoxy) silane, and subsequent treatments such as separation and the like are not needed, so that the yield of the final product vinyl tri (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 rectification, and relates to a method for preparing vinyl tri (beta-methoxyethoxy) silane by catalytic rectification; 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 organic silicon compound, has attracted much attention 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 is widely applied.
The synthesis method of vinyl tri (beta-methoxyethoxy) silane mainly comprises two methods: alcoholysis and transesterification processes.
The alcoholysis method is characterized in that vinyl trichlorosilane and ethylene glycol monomethyl ether are used as raw materials to carry out alcoholysis reaction to synthesize vinyl tri (beta-methoxyethoxy) silane. The by-product obtained by the method is hydrogen chloride gas, and equipment is easy to corrode. The transesterification method is characterized in that vinyl trimethoxy silane and ethylene glycol monomethyl ether are used as raw materials, naOH is used as a catalyst, transesterification reaction is carried out to synthesize vinyl tri (beta-methoxyethoxy) silane, the catalyst is not easy to separate after the reaction is finished, a reaction solution is alkaline, and the purity of a target product is not high.
Disclosure of Invention
The purpose of the invention is as follows: 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 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 reaction section at the middle part and the lower end of the catalytic rectifying tower at the middle 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 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;
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 gathered into a main pipeline through a first arranged pump to be connected to a raw material mixer, and the other end of the raw material mixer is connected to the middle part of a catalytic rectification tower of the catalytic rectification 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, the other end of the first condenser is provided with two connecting pipelines, 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 the methanol product tank;
the tower kettle of the catalytic distillation tower 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 catalytic distillation tower kettle, the other connecting pipeline is connected to a second pump, and the other end of the pump is connected to the middle part of a product distillation tower of the product distillation tower through the installed connecting pipeline;
one end of the top of the product rectifying tower is connected with a second condenser through a connecting pipeline, the other end of the second condenser is provided with two connecting pipelines, one connecting pipeline is connected with the other connecting end of the top of the product rectifying tower, the other connecting pipeline is connected with a raw material tank which is not completely reacted,
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 product rectifying tower kettle, and the other connecting pipeline is connected to the vinyl tri (beta-methoxyethoxy) silane product tank.
Further, the catalytic distillation tower is a packed tower, the height of the packed tower is 2.5m, the height of a distillation section of the catalytic distillation tower is 1m, and the height of a reaction section of the catalytic distillation tower is 1m; the rest is the height of the top of the catalytic rectifying tower, the middle of the catalytic rectifying tower and the height of the bottom of the catalytic rectifying tower;
the product rectifying tower is a packed tower, the height of the packed tower is 3.5m, 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 height of the top of the product rectifying tower, the middle of the product rectifying tower and the height of the bottom of the product rectifying tower.
Further, a method for preparing vinyl tri (beta-methoxyethoxy) silane by using a catalytic rectification reaction device comprises the following specific preparation steps:
firstly, raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are respectively conveyed to a pump through an ethylene glycol monomethyl ether raw material tank and a vinyl trimethoxy silane raw material tank, then conveyed to a raw material mixer through the pump to be mixed, and conveyed to a catalytic rectification tower through a connecting pipeline to be subjected to catalytic rectification reaction after being mixed, so that a byproduct of methanol, a product of vinyl tri (beta-methoxy ethoxy) silane and an unreacted raw material are generated;
secondly, after reaction, evaporating methanol steam from the top of the catalytic distillation tower, sending the methanol steam to a first condenser through a connecting pipeline from the top of the catalytic distillation tower for condensation, wherein part of the methanol steam flows back to the top of the catalytic distillation tower, and the other part of the methanol steam finally enters a methanol product tank through the connecting pipeline;
mixed liquid of raw materials which are not completely reacted and vinyl tri (beta-methoxy ethoxy) silane are taken out from the tower bottom of the catalytic rectification tower and sent to a first reboiler for heating through a connecting pipeline,
after being heated by a reboiler, one part of the waste gas is returned to the bottom of the catalytic distillation tower, and the other part of the waste gas enters a second pump through a connecting pipeline;
finally, the mixed liquid of the unreacted raw material and the vinyl tri (beta-methoxyethoxy) silane entering the second pump is pumped into a product rectifying tower through a connecting pipeline for separation, the unreacted raw material steam is evaporated from the top of the product rectifying tower and is conveyed to a second condenser through the connecting pipeline for condensation, after condensation, one part of the steam flows back to the top of the product rectifying tower, and the other part of the steam flows into a raw material tank which is not completely reacted through the connecting pipeline;
and the product of the vinyl tri (beta-methoxyethoxy) silane is taken out from the tower bottom of the product rectifying tower and heated by the second reboiler, wherein one part of the product of the vinyl tri (beta-methoxyethoxy) silane flows back to the tower bottom of the product rectifying tower, and the other part of the product of the vinyl tri (beta-methoxyethoxy) silane is conveyed to a product tank of the vinyl tri (beta-methoxyethoxy) silane through a connecting pipeline.
Further, the feeding molar ratio of the vinyltrimethoxysilane to the ethylene glycol monomethyl ether is 1:2 to 1:4.
furthermore, the pressure of the catalytic rectifying tower is 0.8-1 MPa, and the reflux ratio of the catalytic rectifying tower is 1-5.
Further, the temperature of the top of the catalytic rectifying tower is 55-65 ℃;
the temperature of the tower kettle of the catalytic distillation tower is 120-140 ℃;
the temperature of the reaction section of the catalytic distillation tower is 90-120 ℃.
Further, a solid base catalyst is filled in the reaction section of the catalytic rectification 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 polyester cloth small bag and then fixed by stainless steel wire mesh corrugated filler;
the catalytic rectifying tower is a packed tower, and the packing of the catalytic rectifying tower is stainless steel wire mesh corrugated packing, wherein only the packing is arranged in the rectifying section of the catalytic rectifying tower, and the catalyst is fixed in the packing in the reaction section of the catalytic rectifying tower.
Furthermore, the operating pressure of the product rectifying tower is 0.18-0.2 MPa absolute pressure, and the reflux ratio of the product rectifying tower is 2-4.
Further, 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 the rectifying section and the stripping section of the product rectifying tower are both provided with stainless steel wire mesh corrugated packing.
The beneficial effects of the invention are: the method for preparing the 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 the product are effectively improved, and meanwhile, the reaction heat is fully utilized, so that the distillation energy consumption is reduced; large-scale continuous production can be realized by adopting continuous catalytic distillation, 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 a liquid product, has higher activity and selectivity and longer catalytic life; meanwhile, the phenomenon of serious corrosion of equipment is relieved, the catalyst adopts a filling technology, the separation difficulty is reduced, the catalyst can be recycled, the cost is reduced, resources are saved, and good economic benefits are created; compared with the prior art, the method has the characteristics of simple process, easy operation, small hazard, high safety, reasonable device structure, low equipment investment, low energy consumption, high conversion rate, high product purity and the like. The advantages brought by the invention are the indexes achieved.
Drawings
FIG. 1 is a schematic view of a catalytic distillation reaction apparatus according to 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 rectifying section of a catalytic rectifying tower, 6 is a reaction section of the catalytic rectifying tower, 7 is a reboiler, 8 is a methanol product tank, 9 is a pump, 10 is a rectifying section of a product rectifying tower, 11 is a stripping section of the product rectifying tower, 12 is a raw material tank which is not completely reacted, and 13 is a vinyl tri (beta-methoxyethoxy) silane product tank.
Detailed Description
The present invention is further described in detail below with reference to examples, it should be noted that the scope of the present invention is not limited to the following examples, which are given for illustrative purposes only and do not limit the present invention in any way.
As shown in the figure, the catalytic distillation tower sequentially comprises a catalytic distillation tower top, a catalytic distillation tower rectifying section (5), a catalytic distillation tower middle part, a catalytic distillation tower reaction section (6) and a catalytic distillation tower kettle from top to bottom;
the material of the rectifying section (5) of the catalytic rectifying tower and the material of the reaction section (6) of the catalytic rectifying tower are stainless steel 304, the inner diameter of the stainless steel is 260mm, the filler is wire mesh corrugated filler, the height of the catalytic rectifying tower is 2m, the number of theoretical plates is about 10, wherein the height of the rectifying section (5) of the catalytic rectifying tower is 1m, the number of theoretical plates is about 5, the height of the reaction section (6) of the catalytic rectifying tower is 1m, the solid base catalyst in the reaction section (6) of the catalytic rectifying tower is K2CO3/Al2O3, the filler is wire mesh corrugations (500, BX), and the solid base catalyst and the wire mesh corrugated filler are mixed by 1:2, the catalyst is uniformly distributed on the surface of the wire mesh corrugated packing and is fixed, and then the catalyst is loaded into a reaction section (6) of a catalytic rectification tower (from top to bottom, 5 th to 10 th theoretical plates).
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 material adopted by the rectifying section (10) of the product rectifying tower and the stripping section (11) of the product rectifying tower is stainless steel 304, the inner diameter is 220mm, the height of the product rectifying tower is 3.5m, the height of the rectifying section (10) of the product rectifying tower is 1.4m, and the height of the stripping section (11) of the product rectifying tower is 1.6m; the number of theoretical plates of the rectifying section (10) of the product rectifying tower is about 7, and the number of theoretical plates of the stripping section (11) of the product rectifying tower is about 8.
The gas chromatographic analysis of the product was as follows: SE-54 (30m 0.32mm 0.50um) capillary chromatography column, FID hydrogen flame detector; the initial temperature is 130 ℃, the temperature is kept for 1min, the final temperature is 280 ℃, the temperature is kept for 8min, and the heating rate is 15 ℃ min < -1 >; the detector temperature is 300 ℃, the vaporization chamber temperature is 300 ℃, the carrier gas flow rate is 40 mL/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 (3) through the pump (9) to be mixed, and conveyed to the middle part of a catalytic rectification tower through a connecting pipeline after being mixed, and then enters the catalytic rectification tower from the middle part of the catalytic rectification tower through the pump, wherein the ethylene glycol monomethyl ether and the vinyl trimethoxy silane perform countercurrent heat and mass transfer in a reaction section of the catalytic rectification tower, and perform ester exchange reaction under the action of a solid base catalyst in the reaction section (6) of the catalytic rectification tower; after ethylene glycol monomethyl ether and vinyl trimethoxy silane react, high-purity methanol is arranged at the top of the tower, and a mixed solution of raw materials which do not completely react and vinyl tri (beta-methoxyethoxy) silane is arranged at the bottom of the tower; separating the raw material which is not completely reacted and the vinyl tri (beta-methoxyethoxy) silane mixed solution by a product rectifying tower, and then extracting the vinyl tri (beta-methoxyethoxy) silane with higher purity from the tower kettle.
Example 1
By adopting the process flow shown in the attached figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are mixed in a ratio of 3:1, feeding the raw materials at normal temperature, wherein the flow of ethylene glycol monomethyl ether is 91.3kg/h, the flow of vinyl trimethoxy silane is 59.3kg/h, respectively feeding the raw materials from respective raw material storage tanks into the 5 th plate of a rectifying section (5) of a catalytic rectifying tower through a pump (9), the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 97 ℃, the temperature of the top of the catalytic rectifying tower is stabilized to be 58.7 ℃, the temperature of the bottom of the catalytic rectifying tower is stabilized to be 135.8 ℃, controlling the reflux ratio of the top of the catalytic rectifying tower to be 4; through gas phase analysis, the yield of the catalytic rectifying tower product is 60%, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is 99.2%.
Example 2
By adopting the process flow shown in the attached figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are mixed in a ratio of 3.5:1, feeding the raw materials 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 raw materials from respective raw material storage tanks into the 5 th plate of a rectifying section (5) of a catalytic rectifying tower through a pump (9), the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 99 ℃, the temperature of the top of the catalytic rectifying tower is stabilized to be 62 ℃, the temperature of the bottom of the catalytic rectifying tower is stabilized to be 135.7 ℃, controlling the reflux ratio to be 4; the gas phase analysis found that the yield of the catalytic distillation column product was 78% and the purity of the distillation column product, vinyltris (. Beta. -methoxyethoxy) silane, was 99.5%.
Example 3
By adopting the process flow shown in the attached figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are mixed in a ratio of 4:1, 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 raw materials from respective raw material storage tanks into the 5 th plate of a rectifying section (5) of a catalytic rectifying tower through a pump, controlling the pressure of the catalytic rectifying tower to be 0.8MPa, the reaction temperature to be 100 ℃, the temperature of the top of the catalytic rectifying tower to be 65 ℃, the temperature of the bottom of the catalytic rectifying tower to be 135.5 ℃, controlling the reflux ratio to be 4; after the reaction, the gas phase analysis shows that the yield of the catalytic rectifying tower product is 80 percent, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is 99.8 percent.
Comparative example 1
By adopting the process flow shown in the attached figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are mixed in a ratio of 4:1, 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 raw materials from respective raw material storage tanks into the 5 th plate of a rectifying section (5) of a catalytic rectifying tower through a pump, controlling the reflux ratio to be 0, and pumping the raw materials and the products which are not completely reacted in the tower bottom of the catalytic rectifying tower into a product rectifying tower for separation, wherein the pressure of the catalytic rectifying tower is 0.8MPa, the reaction temperature is 100 ℃, the temperature of the tower top of the catalytic rectifying tower is stabilized to be 65 ℃, the temperature of the tower bottom of the catalytic rectifying tower is stabilized to be 135.5 ℃; after the reaction, gas phase analysis shows that the yield of the catalytic rectifying tower product is 50%, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is 90%.
Comparative example 2
By adopting the process flow shown in the attached figure 1, the raw materials of ethylene glycol monomethyl ether and vinyl trimethoxy silane are mixed in a ratio of 4:1, 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 from respective raw material storage tanks into the 5 th plate of a catalytic rectification tower rectification section (5), and compared with the implementation of 1-3, not filling a solid base catalyst in a catalytic rectification tower reaction section (6), controlling the pressure of the catalytic rectification tower to be 0.8MPa, the reaction temperature to be 100 ℃, the temperature of the top of the catalytic rectification tower to be 65 ℃, the temperature of the bottom of the catalytic rectification tower to be 135.5 ℃, controlling the reflux ratio to be 4; after the reaction, the gas phase analysis shows that the yield of the catalytic rectifying tower product is 45 percent, and the purity of the rectifying tower product vinyl tri (beta-methoxyethoxy) silane is 87 percent.
Finally, it should be understood that the embodiments described herein are merely illustrative of the principles of embodiments of the present invention; other variations are possible within the scope of the invention; accordingly, the embodiments of the invention are not limited to the embodiments explicitly described and depicted.
Claims (9)
1. A catalytic rectification reaction device is characterized in that: 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, a raw material tank (12) which does not react completely 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 part and the lower end of the catalytic rectifying tower at the middle end, 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 part and the lower end of the product rectifying tower at the middle end, 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 gathered into a main pipeline through a first arranged pump (9) to be connected onto a raw material mixer (3), and the other end of the raw material mixer (3) is connected onto the middle part of a catalytic rectification tower of the catalytic rectification tower through the arranged connecting pipelines;
one end of the top of the catalytic distillation tower is connected to a first condenser (4) through a connecting pipeline, the other end of the first condenser (4) is provided with two connecting pipelines, one connecting pipeline is connected to the other end of the top of the catalytic distillation tower, and the other connecting pipeline is connected to a methanol product tank (8);
the bottom of the catalytic distillation 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 of the connecting pipelines is connected to the other end of the catalytic distillation tower kettle, the other connecting pipeline is connected to the second pump (9), and the other end of the pump (9) is connected to the middle part of a product distillation tower of the product distillation tower through the installed connecting pipeline;
one end of the top of the product rectifying tower is connected with a second condenser (4) through a connecting pipeline, the other end of the second condenser (4) is provided with two connecting pipelines, one connecting pipeline is connected with the other connecting end of the top of the product rectifying tower, the other connecting pipeline is connected with a raw material tank (12) which is not completely reacted,
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 product rectifying tower kettle, and the other connecting pipeline is connected to the vinyl tri (beta-methoxyethoxy) silane product tank (13).
2. The method for preparing vinyltri (beta-methoxyethoxy) silane according to claim 1, wherein,
the catalytic distillation tower is a packed tower, the height of the packed tower is 2.5m, the height of a distillation section (5) of the catalytic distillation tower is 1m, and the height of a reaction section (6) of the catalytic distillation 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.
3. The method for preparing vinyl tri (beta-methoxyethoxy) silane by using the catalytic distillation reaction device as claimed in any of claims 1 to 2, which 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) to be mixed, and conveyed into a catalytic rectifying tower through a connecting pipeline to be subjected to catalytic rectifying reaction after being mixed, so that a byproduct of methanol, a product of vinyl tri (beta-methoxyethoxy) silane and unreacted raw materials are generated;
secondly, after reaction, methanol steam is distilled from the top of the catalytic distillation tower, and is sent to a first condenser (4) through a connecting pipeline to be condensed through the top of the catalytic distillation tower, wherein part of the methanol steam flows back to the top of the catalytic distillation tower, and the other part of the methanol steam finally enters a methanol product tank (8) through the connecting pipeline;
mixed liquid of raw materials which are not completely reacted and vinyl tri (beta-methoxyethoxy) silane are taken out from the tower bottom of the catalytic rectification tower and sent to a first reboiler (7) through a connecting pipeline for heating,
after being heated by a reboiler (7), one part of the waste water is returned to the bottom of the catalytic distillation tower, and the other part of the waste water enters a second pump (9) through a connecting pipeline;
finally, the mixed liquid of the raw material which is not completely reacted and the vinyl tri (beta-methoxyethoxy) silane which enter the second pump (9) is pumped into a product rectifying tower through a connecting pipeline for separation, the raw material steam which is not completely reacted is evaporated from the top of the product rectifying tower and is conveyed to the second condenser (4) through the connecting pipeline for condensation, after condensation, one part of the condensed raw material flows back to the top of the product rectifying tower, and the other part of the condensed raw material enters a raw material tank (12) which is not completely reacted through the connecting pipeline;
and the product of the vinyltris (beta-methoxyethoxy) silane is taken out from the tower bottom of the product rectifying tower and heated by a second reboiler (7), wherein one part of the vinyltris (beta-methoxyethoxy) silane flows back to the tower bottom of the product rectifying tower, and the other part of the vinyltris (beta-methoxyethoxy) silane is conveyed to a vinyltris (beta-methoxyethoxy) silane product tank (13) through a connecting pipeline.
4. The method for preparing vinyltri (beta-methoxyethoxy) silane by using a catalytic distillation reaction unit according to claim 3,
the feeding molar ratio of the vinyltrimethoxysilane to the ethylene glycol monomethyl ether is 1:2 to 1:4.
5. the method for preparing vinyltri (beta-methoxyethoxy) silane by using a catalytic distillation reaction unit according to claim 3,
the pressure of the catalytic rectifying tower is 0.8-1 MPa, and the reflux ratio of the catalytic rectifying tower is 1-5.
6. The method for preparing vinyltri (beta-methoxyethoxy) silane according to claim 3, wherein,
the temperature of the top of the catalytic rectifying tower is 55-65 ℃;
the temperature of the tower kettle of the catalytic distillation tower is 120-140 ℃;
the temperature of the reaction section (6) of the catalytic rectifying tower is 90-120 ℃.
7. The method for preparing vinyltri (beta-methoxyethoxy) silane by using a catalytic distillation reaction unit according to claim 3,
the reaction section (6) of the catalytic rectification tower is filled with a solid base catalyst, 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 polyester cloth small bag and then fixed by stainless steel wire mesh corrugated filler.
8. The method for preparing vinyltri (beta-methoxyethoxy) silane according to claim 3, wherein,
the operating pressure of the product rectifying tower is 0.18-0.2 MPa absolute pressure, and the reflux ratio of the product rectifying tower is 2-4.
9. The method for preparing vinyltri (beta-methoxyethoxy) silane by using a catalytic distillation reaction unit according to claim 3,
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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