CN114940687A - Continuous flow synthesis method of polysubstituted vinyl silicon (oxy) alkane - Google Patents
Continuous flow synthesis method of polysubstituted vinyl silicon (oxy) alkane Download PDFInfo
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- 150000001335 aliphatic alkanes Chemical class 0.000 title claims abstract description 37
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical class [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000001308 synthesis method Methods 0.000 title description 4
- 238000004519 manufacturing process Methods 0.000 claims abstract description 52
- IJMWREDHKRHWQI-UHFFFAOYSA-M magnesium;ethene;chloride Chemical compound [Mg+2].[Cl-].[CH-]=C IJMWREDHKRHWQI-UHFFFAOYSA-M 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims description 67
- 238000000034 method Methods 0.000 claims description 42
- 239000000758 substrate Substances 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 27
- 239000000047 product Substances 0.000 claims description 25
- 230000035484 reaction time Effects 0.000 claims description 16
- 239000002904 solvent Substances 0.000 claims description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 5
- -1 vinylsilyl (oxy) alkane Chemical class 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims description 3
- 125000005373 siloxane group Chemical group [SiH2](O*)* 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- WDVUXWDZTPZIIE-UHFFFAOYSA-N trichloro(2-trichlorosilylethyl)silane Chemical compound Cl[Si](Cl)(Cl)CC[Si](Cl)(Cl)Cl WDVUXWDZTPZIIE-UHFFFAOYSA-N 0.000 claims description 3
- QHAHOIWVGZZELU-UHFFFAOYSA-N trichloro(trichlorosilyloxy)silane Chemical compound Cl[Si](Cl)(Cl)O[Si](Cl)(Cl)Cl QHAHOIWVGZZELU-UHFFFAOYSA-N 0.000 claims description 3
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
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- 238000010924 continuous production Methods 0.000 description 8
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 239000002000 Electrolyte additive Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001350 alkyl halides Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 229910002110 ceramic alloy Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
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- CPBHJGWJMLDUNB-UHFFFAOYSA-N ethenoxysilane Chemical class [SiH3]OC=C CPBHJGWJMLDUNB-UHFFFAOYSA-N 0.000 description 1
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- 150000004795 grignard reagents Chemical class 0.000 description 1
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- 239000002184 metal Substances 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
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- 238000011112 process operation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001256 stainless steel alloy Inorganic materials 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 150000005672 tetraenes Chemical class 0.000 description 1
- UFHILTCGAOPTOV-UHFFFAOYSA-N tetrakis(ethenyl)silane Chemical compound C=C[Si](C=C)(C=C)C=C UFHILTCGAOPTOV-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0805—Compounds with Si-C or Si-Si linkages comprising only Si, C or H atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0803—Compounds with Si-C or Si-Si linkages
- C07F7/0825—Preparations of compounds not comprising Si-Si or Si-cyano linkages
- C07F7/0827—Syntheses with formation of a Si-C bond
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/0834—Compounds having one or more O-Si linkage
- C07F7/0838—Compounds with one or more Si-O-Si sequences
- C07F7/0872—Preparation and treatment thereof
- C07F7/0876—Reactions involving the formation of bonds to a Si atom of a Si-O-Si sequence other than a bond of the Si-O-Si linkage
- C07F7/0878—Si-C bond
Abstract
The invention provides a full continuous flow production method of polysubstituted vinyl silicon (oxy) alkane, the production process is carried out in an integrated continuous flow reactor, raw materials such as vinyl magnesium chloride and the like are uninterruptedly added into a feed inlet of the integrated continuous flow reactor, and the polysubstituted vinyl silicon (oxy) alkane is uninterruptedly obtained at a discharge outlet of the integrated continuous flow reactor. Compared with the traditional production process, the production time is shortened to be within 5 minutes, no amplification effect is generated, the selectivity is good, the yield is high, the product index is stable, and the reproducibility is good.
Description
Technical Field
The invention relates to the field of chemistry, in particular to a full continuous flow production method for preparing polysubstituted vinyl silicon (oxy) alkane.
Background
Polysubstituted vinyl silicon (oxy) alkane is a very important chemical raw material, such as tetravinyl silane, which is a very important electrolyte additive, and the current synthesis method of polysubstituted vinyl silicon (oxy) alkane generally adopts a direct method and an organic metal synthesis method. The direct method is that vinyl-containing alkyl halide and different chloro-sila (oxy) alkane are directly reacted under the action of copper catalyst and higher temperature to obtain the product. Organometallic methods generally employ grignard reagents and are the most widely used.
The prior art of polysubstituted vinyl silicon (oxy) alkane has a plurality of problems: the existing process can not effectively inhibit the generation of impurities, so that the product quality is poor and the yield is low; amplification effects of different degrees exist, so that a large amount of manpower and material resources are consumed and a plurality of uncertainties exist when the amplification is carried out to industrialization; the use of hazardous raw material vinyl magnesium chloride presents certain safety risks; the existing process has overlong reaction time, greatly reduces the production efficiency, and increases the difficulty of industrialization. But the application is limited because the large-scale production can not be realized. Therefore, a continuous flow production process of polysubstituted vinyl (oxy) silane, which is simple and safe to operate, efficient, easy to produce on a large scale and free of amplification effect, is needed.
The continuous production process refers to the fact that production steps of a production system are mutually connected in the production process, the continuous operation is guaranteed on the whole, and the continuous production process is allowed to stay and wait in each step. The continuous flow production process is one kind of continuous process, is one fast and efficient full-flow continuous process, has the features of short time consumption, high efficiency, easy operation, etc. the continuous production process has continuous material feeding, continuous product production, continuous flowing of material, no interruption and no stay, and is one kind of "assembly line" type chemical production process. When the process operation reaches a steady state, the state parameters of the material composition, the temperature and the like at any position in the reactor do not change along with the time, and the process is a steady state process, so the production process and the product quality are stable. In a process involving multiple reactions, if some of the steps are continuous or simply connected, the process may be referred to as a semi-continuous process; rather, a continuous flow process (or a full flow continuous process) is only possible if all steps are continuous and the material flows continuously throughout the process, i.e., the feed is continuously added and the product is continuously obtained.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a full continuous flow production method of polysubstituted vinyl silicon (oxy) alkane, which has the advantages of simple and safe operation, high efficiency, no amplification effect and the like, and the prepared polysubstituted vinyl silicon (oxy) alkane has high yield and content, stable quality and easy large-scale production, greatly reduces the production cost and improves the production safety of the polysubstituted vinyl silicon (oxy) alkane.
The technical scheme adopted by the invention is as follows:
a full continuous flow production method for preparing polysubstituted vinyl silicon (oxy) alkane comprises the following steps:
continuously adding vinyl magnesium chloride and reaction substrates into the integrated continuous flow reactor according to a ratio to react, continuously obtaining a product from a discharge port of the integrated continuous flow reactor, and separating and purifying the product to obtain polysubstituted vinyl silane (oxy) alkane; wherein the reaction temperature in the integrated continuous flow reactor is 0-50 ℃, and the reaction time is 2-5 min; the integrated continuous flow reactor is composed of one or more micro reactor modules or micro reactor module groups; the reaction substrate contains silane or siloxane groups, and the micro reactor module group is formed by connecting a plurality of micro reactor modules in series or in parallel.
The production time of the process is less than or equal to 5 min. The production time refers to the time (equal to the reaction time of the reaction raw materials in the integrated continuous flow reactor) from the time when the reaction raw materials (the vinyl magnesium chloride and the reaction substrates) enter the integrated continuous flow reactor to the time when the target product is output.
Further, the yield of the polysubstituted vinyl silicon (oxy) alkane is more than or equal to 50 percent; preferably, the yield of the polysubstituted vinyl silicon (oxy) alkane is more than or equal to 60 percent; more preferably, the yield of the polysubstituted vinylsilyl (oxy) alkane is not less than 70%.
Further, the content of the polysubstituted vinyl silicon (oxy) alkane is more than or equal to 95 percent; preferably, the content of the polysubstituted vinyl silicon (oxy) alkane is more than or equal to 97 percent; the content of the polysubstituted vinyl silicon (oxy) alkane is more than or equal to 99 percent.
Further, the reaction temperature is 0-50 ℃, preferably 0-40 ℃, and more preferably 5-30 ℃.
Further, the reaction substrate is preferably tetrachlorosilane, 1, 2-bis (trichlorosilyl) methane, hexachlorodisiloxane, 1, 2-bis (trichlorosilyl) ethane.
The invention uses the super-strong mixing micro-reactor, can achieve excellent mixing effect in a very short time, ensures that the vinyl magnesium chloride and the reaction substrate are uniformly dispersed, and the vinyl magnesium chloride and the reaction substrate are contacted in proportion in the reaction process, and simultaneously, the reaction can be completed in a very short time by matching the module combination and the temperature zone, thereby greatly avoiding the generation of impurities and improving the production efficiency.
The solution of the invention has no amplification effect, thus greatly reducing the difficulty of industrial application, and when the solution is amplified to the industrialization, the required production scale can be amplified once without complicated multiple step-by-step amplification and adjustment and optimization of process conditions and parameters, thereby greatly saving manpower, material resources and project development time; in industrial production, the production scale of the product can be flexibly changed, the process conditions and parameters do not need to be readjusted and optimized, and the flexibility of the production process is good; the production process is stable and reliable due to no amplification effect, the product quality is not influenced by the fluctuation of process conditions and parameters, and the product quality is easy to control; this also greatly improves the safety of the production process.
The continuous flow process of the invention has good stability and reliability, so the product quality is stable and the reproducibility is good; meanwhile, the production time is short, the size is small, the occupied area is small, the land for a factory building is greatly saved, and the production efficiency is improved.
The production process can continuously complete the reaction for preparing the polysubstituted vinyl silicon (oxy) alkane in a very short time, and by utilizing the functional unit division, the optimization of temperature setting and the synergistic effect of the functional units, the total reaction time can be shortened to be within 5min, so that the process efficiency is greatly improved. Therefore, the production process breaks through the limitation of the prior art, successfully realizes the high-efficiency and high-quality production of the polysubstituted vinyl silicon (oxy) alkane, and is a great breakthrough in the field.
Further, in order to match with the full continuous flow production process of the polysubstituted vinyl silicon (oxy) alkane, the integrated continuous flow reactor adopts a unitized structure and comprises a pre-reaction unit and a curing unit, wherein: comprising a pretreatment unit and a curing unit, wherein: the pretreatment unit is used for realizing mixed pre-reaction of a reaction substrate and vinyl magnesium chloride, and the curing unit is used for complete reaction of the polysubstituted vinyl silicon (oxy) alkane.
Further, the temperature of the pre-reaction unit is 0-10 ℃, and preferably 0-5 ℃.
Further, the temperature of the curing unit is 0-50 ℃, preferably 5-40 ℃, and more preferably 10-30 ℃.
Further, for matching with the full continuous flow production process of the polysubstituted vinyl silicon (oxy) alkane, each unit independently comprises more than one reactor module or reactor module group, wherein the reactor module group is formed by connecting a plurality of reactor modules in series or in parallel, and the units are connected in series.
Furthermore, each unit comprises at least one temperature zone, and each temperature zone independently comprises one or more micro-reactor modules or reactor module groups.
Further, the number of the feeding ports of the integrated continuous flow reactor is 1 or more, and the number of the discharging ports of the integrated continuous flow reactor is 1 or more.
Further, the number of reactors may be one or more.
Furthermore, the material of the reactor channel is monocrystalline silicon, special glass, ceramic, stainless steel or metal alloy coated with a corrosion-resistant coating, and polytetrafluoroethylene.
Furthermore, the reactor modules, the reactor module groups and the reactor modules and the reactor module groups are respectively connected in series or in parallel.
Further, the continuous flow production process is carried out in an integrated continuous flow reactor comprising 2 temperature zones.
Further, the pre-reaction unit of the continuous flow production process comprises 1 temperature zone which is a temperature zone 1, and the curing unit comprises 1 temperature zone which is a temperature zone 2.
Further, the continuous flow production process comprises the following steps:
(a) the vinylmagnesium chloride and the reaction substrate are conveyed into a pre-reaction unit, passing through a temperature zone 1.
(b) And (3) allowing the reaction liquid flowing out of the temperature zone 1 to enter a curing unit, curing through the temperature zone 2, and separating and purifying to obtain a target product.
Further, the temperature of the temperature zone 1 is 0-10 ℃, preferably 0-5 ℃.
Further, the temperature of the temperature zone 2 is 0-50 ℃, preferably 5-40 ℃, and more preferably 10-30 ℃.
Further, the concentration of the vinyl magnesium chloride and the reaction substrate is 20 wt% to 50 wt%, preferably 30 wt% to 50 wt%, more preferably 40 wt% to 50 wt%, and the solvent is tetrahydrofuran.
Further, the flow rate of the vinylmagnesium chloride and the reaction substrate is 20 to 300g/min, preferably 50 to 260g/min, and more preferably 50 to 170 g/min.
Further, the method for separating and purifying the product comprises the following steps: distilling under reduced pressure at 40 deg.C to remove solvent and salt, filtering to remove salt, introducing the filtrate into rectifying column, distilling at 70 deg.C to remove solvent, and distilling at 120 deg.C to obtain polysubstituted vinylsilyl (oxy) alkane.
The invention provides a scheme for directly and continuously producing polysubstituted vinyl silicon (oxy) alkane from reaction substrates, namely, a plurality of reactants are continuously input into a reactor, and reaction products are continuously collected. By means of the temperature zone division and temperature setting optimization of the functional units and the synergistic effect of the functional units, the full reaction can be realized in a short time, the total reaction time is shortened to be within 5min, and the process efficiency is greatly improved.
The continuous flow process has good stability and reliability, so the product quality is stable and the reproducibility is good; the process has no amplification effect, and also solves the problem of amplification effect in the industrialization of the continuous flow process of the polysubstituted vinyl silicon (oxy) alkane; meanwhile, the integrated continuous flow reactor does not need a delay pipeline, so that the integrated continuous flow reactor is small in size and small in occupied area, and the land for a factory building is greatly saved.
Compared with the prior art, the invention has the following beneficial effects:
1. the production process of the invention is to directly prepare the product within a short time (within 5 min), the production process is safe and efficient, the yield and the content of the prepared polysubstituted vinyl silicon (oxy) alkane product are high, the generation of impurities is effectively controlled, the production cost is greatly reduced, and the production efficiency and the safety are improved.
2. The method solves the problem of industrial amplification of the continuous flow process of the polysubstituted vinyl silicon (oxy) alkane, has no amplification effect, greatly reduces the difficulty of industrial application, can be amplified to the required production scale once without complicated multiple step-by-step amplification and adjustment and optimization of process conditions and parameters during industrial amplification, and greatly saves manpower, material resources and project development time.
3. The safety of the production process is greatly improved, the relatively small liquid holdup and excellent heat transfer characteristic of the continuous flow reactor are realized, and the process is safer due to the short reaction time (within 5 min).
4. Compared with the prior art, the method has the advantages that the reaction time is greatly shortened by more than 50%, and the reaction efficiency is greatly improved.
5. The integrated continuous flow reactor has small volume and small occupied area, and greatly saves the land for a factory building.
Drawings
FIG. 1 is a schematic view of an integrated reactor according to the present invention;
FIG. 2 is a process diagram of the continuous production process of the present invention;
FIG. 3 is a hydrogen spectrum of synthesized tetraene silicon.
Detailed Description
The invention provides a full continuous flow production method for preparing polysubstituted vinyl silicon (oxy) alkane, as shown in figure 2, which specifically comprises the following steps:
continuously adding vinyl magnesium chloride and reaction substrates into the integrated continuous flow reactor in proportion for reaction, continuously obtaining products from a discharge port of the integrated continuous flow reactor, and separating and purifying the products to obtain polysubstituted vinyl silane (oxy) alkane; wherein the reaction temperature in the integrated continuous flow reactor is 0-50 ℃, and the reaction time is 2-5 min; the system consists of one or more micro reactor modules or micro reactor module groups; the reaction substrate contains silane or siloxane groups, and the micro reactor module group is formed by connecting a plurality of micro reactor modules in series or in parallel.
The production process of the invention has the following reaction formula:
wherein the reaction substrate is one or more of tetrachlorosilane, 1, 2-bis (trichlorosilyl) methane, hexachlorodisiloxane and 1, 2-bis (trichlorosilyl) ethane.
The flow rate of the vinyl magnesium chloride and the reaction substrate is 20-300g/min, and the solvent is tetrahydrofuran.
The production method of the invention prepares polysubstituted vinyl silicon (oxy) alkane continuously under the condition of strictly controlling the proportion of the vinyl magnesium chloride and the reaction substrate, the production process is carried out in an integrated continuous flow reactor, continuously adding reaction substrates and vinyl magnesium chloride into a feed inlet of the integrated continuous flow reactor, continuously obtaining the polysubstituted vinyl silicon (oxygen) alkane of the target product at the discharge hole of the integrated continuous flow reactor, the integrated continuous flow reactor has an incomparable super-strong mixing effect compared with the traditional process, so that the vinyl magnesium chloride and the reaction substrate can achieve an excellent mixing effect in a very short time, the vinyl magnesium chloride and the reaction substrate are uniformly dispersed, the vinyl magnesium chloride and the reaction substrate are contacted in proportion in the reaction process, can be finished in a very short time, greatly avoids the generation of impurities and improves the production efficiency.
Further, to meet the conditions of the continuous flow process of the present invention, the present invention optimizes the module combinations and temperature zones of the integrated reactor: by utilizing the functional unit division, the optimization of temperature setting and the synergistic effect of the functional units, the total reaction time can be shortened to within 5min, and the efficiency of the process is further improved. The optimization of module combination and temperature zones requires the design of the organization and number of modules, the modules contained in each temperature zone, and the development of targeted process conditions and parameters, including the synergistic effect of various factors such as the division of each temperature zone and the temperature setting, so that the continuous flow process is realized. And the temperature, the material concentration, the material ratio and the material flow rate can be further combined to be matched with the reaction process, so that a better reaction effect is obtained. The specific implementation is as follows:
in order to match with the full continuous flow production process of the polysubstituted vinyl silicon (oxy) alkane, the integrated continuous flow reactor adopts a unitized structure, each unit comprises at least one temperature zone, each temperature zone independently comprises more than one reactor module or reactor module group, the reactor module group is formed by connecting a plurality of reactor modules in series or in parallel, and the temperature zones are connected in series with each other.
Further, the integrated continuous flow reactor is formed by connecting two units in series, wherein the first unit is a pre-reaction unit for realizing the mixed pre-reaction of reaction substrates and vinyl magnesium chloride, and the second unit is a curing unit for the complete reaction of the polysubstituted vinyl silicon (oxy) alkane. The pre-reaction unit comprises a temperature zone with the temperature of 0-10 ℃ and the reaction time of 20s-1min, and the curing unit comprises a temperature zone with the temperature of 0-50 ℃ and the reaction time of 2-4 min.
The vinyl magnesium chloride and the reaction substrate are mixed and pre-reacted in a temperature zone 1, and then enter a temperature zone 2 to continuously and completely react to obtain the polysubstituted vinyl silicon (oxy) alkane.
More preferably, the pre-reaction unit comprises a temperature zone with the temperature of 0-5 ℃ and the reaction time of 20s-1min, and the curing unit comprises a temperature zone with the temperature of 5-40 ℃ and the reaction time of 2-4 min.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
As shown in fig. 1 and fig. 2, the raw material 1 and the raw material 2 are sequentially conveyed to an integrated continuous flow reactor by a constant flow pump, and sequentially enter a temperature region 1 to a temperature region 2, the reaction is complete, and the product is obtained after rectification, wherein the rectification process specifically comprises the following steps: most of the solvent was distilled off under reduced pressure at 40 ℃ with a large amount of salt being precipitated, and filtered. The filtrate was passed through a rectification column, the solvent was still distilled off at a vapor temperature of 70 ℃ and the product was distilled off at a vapor temperature of 120 ℃, and FIG. 3 is a hydrogen spectrum of the hydrogen spectrum of tetraethenosilane synthesized in example 5. The reaction conditions and results of each example and comparative example are shown in the following table, in which feed rate 1 represents the feed rate of vinylmagnesium chloride and feed rate 2 represents the feed rate of the reaction substrate.
It should be noted that, the reaction substrate and the vinyl magnesium chloride used in the actual production (including the laboratory, the pilot plant test and the actual production process) have the deviation of mass concentration of plus or minus 2 percentage points; the temperature of the temperature zone has deviation of +/-3 ℃; the production time may vary by + -5 s.
Comparing examples 1-8 with the comparative example, it can be seen that when the reaction temperature in the integrated continuous flow reactor is 0-50 ℃, the reaction for preparing polysubstituted vinyl silicon (oxy) alkane can be continuously completed in a very short time, thereby realizing high yield, avoiding the generation of impurities and improving the production efficiency.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. This need not be, nor should all embodiments be exhaustive. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (10)
1. A full continuous flow production method for preparing polysubstituted vinyl silicon (oxy) alkane is characterized by comprising the following steps:
continuously adding vinyl magnesium chloride and reaction substrates into the integrated continuous flow reactor in proportion for reaction, continuously obtaining products from a discharge port of the integrated continuous flow reactor, and separating and purifying the products to obtain polysubstituted vinyl silane (oxy) alkane; wherein the reaction temperature in the integrated continuous flow reactor is 0-50 ℃, and the reaction time is 2-5 min; the integrated continuous flow reactor consists of one or more micro reactor modules or micro reactor module groups; the reaction substrate contains silane or siloxane groups, and the micro reactor module group is formed by connecting a plurality of micro reactor modules in series or in parallel.
2. The method of claim 1, wherein the reaction substrate is one or more of tetrachlorosilane, 1, 2-bis (trichlorosilyl) methane, hexachlorodisiloxane, 1, 2-bis (trichlorosilyl) ethane.
3. The method of claim 1, wherein the integrated continuous flow reactor is comprised of 1 or more connected units, each unit comprising at least one temperature zone, each temperature zone independently comprising one or more microreactor modules or groups of reactor modules.
4. The method according to claim 3, wherein the integrated continuous flow reactor is composed of two units connected together, wherein the first unit is a pre-reaction unit and the second unit is a curing unit, the pre-reaction unit comprises a temperature zone with the temperature of 0-10 ℃ and the reaction time of 20s-1min, the curing unit comprises a temperature zone with the temperature of 0-50 ℃ and the reaction time of 2-4 min.
5. The method according to claim 4, wherein the pre-reaction unit comprises a temperature zone having a temperature of 0 to 5 ℃, and the curing unit comprises a temperature zone having a temperature of 5 to 40 ℃.
6. The process of claim 1, wherein the vinyl magnesium chloride and reaction substrate flow rates are in the range of 20 to 300 g/min.
7. The method of claim 6, wherein the vinyl magnesium chloride and the reaction substrate flow rate is 50 to 170 g/min.
8. The method of claim 1, wherein the concentration of vinyl magnesium chloride and reaction substrate is 20 wt% to 50 wt%.
9. The method of claim 1, wherein the concentration of the vinyl magnesium chloride and the reaction substrate is 30 wt% to 50 wt%, and the solvent is tetrahydrofuran.
10. The method according to claim 1, wherein the method for separating and purifying the product comprises: distilling under reduced pressure at 40 deg.C to remove solvent and salt, filtering to remove salt, introducing the filtrate into rectifying column, distilling at 70 deg.C to remove solvent, and distilling at 120 deg.C to obtain polysubstituted vinylsilyl (oxy) alkane.
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