Vinyltrichlorosilane and production method and system thereof

Abstract

The present invention provides vinyl trichlorosilane and a production method and system thereof. The production method comprises: a portion of a solvent and catalyst mixture in a reactor is input into a venturi mixer to generate a vacuum therein, and raw materials for producing vinyl trichlorosilane are introduced into the venturi mixer to mix with the solvent and catalyst entering therein, and the formed gas-liquid two-phase mixture is discharged into a reaction tube located in the reactor and connected to the venturi mixer during the pressure relief process of the venturi mixer, and under the reaction conditions provided by the reactor, the production raw materials in the gas-liquid two-phase mixture react under the action of the catalyst to generate a reaction product, vinyl trichlorosilane, and at the same time, the reaction product generated due to the pressure relief effect of the venturi mixer is flashed to form saturated steam to escape from the reaction tube, thereby avoiding the side reaction between the reaction product and the raw material trichlorosilane, and greatly reducing the generation of by-products. The catalyst and solvent in the reaction tube are returned to the reactor.

Description

Technical Field

[0001] The present invention particularly relates to vinyltrichlorosilane and a production method and system thereof. Background Art

[0002] Vinyl trichlorosilane is a kind of organosilicon silane coupling agent, and its molecular formula is CH2=CHSiCl3. Because it has unsaturated groups and active chlorine radicals, it hydrolyzes violently in water to form corresponding silanols. It is suitable for use as a surface treatment agent for glass fiber and a treatment agent for reinforced plastic laminates to improve the mechanical strength, heat resistance and moisture resistance of the products. It can also be used as a raw material for other vinyl organosilicon coupling agents. It is also suitable for the surface treatment of glass fiber, and can improve the adhesion, heat resistance and water resistance of glass fiber with unsaturated polyester, epoxy resin, acrylic resin, etc.

[0003] At present, the main production process route is the addition reaction of acetylene and trichlorosilane under the catalysis of chloroplatinic acid to generate vinyltrichlorosilane. According to the reaction process, it is mainly classified into kettle reaction and tower reaction. Both reaction processes use chloroplatinic acid and ligand as catalysts to obtain the corresponding target product.

[0004] The current kettle reaction mainly involves inserting acetylene gas and trichlorosilane gas into the reactor from the raw material addition port through a tube, and reacting in a solvent with a catalyst. Chlorobenzene or xylene is generally selected as the solvent. Patent CN 211677751 U mentions the use of stirring to accelerate the reaction efficiency and the efficiency of removing the reaction heat. Patent CN212092218 U mentions the use of a distributor in the reactor, and the vaporized gases of acetylene and trichlorosilane enter the distributor to increase the reaction contact area and the uniformity of the reaction raw materials. The above-mentioned existing vinyl trichlorosilane reactor mainly has the following defects: vinyl trichlorosilane is very easy to react with trichlorosilane in the raw material under the temperature of vinyl trichlorosilane generation and the action of the catalyst, resulting in high by-products and high catalyst unit consumption. Summary of the invention

[0005] The technical problem to be solved by the present invention is to provide a method for producing vinyltrichlorosilane with reduced by-products and improved yield in view of the above-mentioned deficiencies in the prior art, and also provide vinyltrichlorosilane prepared by the method and a system corresponding to the method.

[0006] The technical solution adopted to solve the technical problem of the present invention is:

[0007] The present invention provides a method for producing vinyltrichlorosilane, comprising:

[0008] A portion of the solvent and catalyst mixture in the reaction kettle is introduced into a venturi mixer to generate a vacuum in the venturi mixer and a raw material for producing vinyltrichlorosilane is introduced into the venturi mixer to mix with the solvent and catalyst entering the venturi mixer to form a gas-liquid two-phase mixture,

[0009] The gas-liquid two-phase mixture is discharged into a reaction tube located in the reaction kettle and connected to the Venturi mixer during the pressure relief process of the Venturi mixer.

[0010] Under the reaction conditions provided by the reactor, the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst to generate a reaction product, vinyltrichlorosilane.

[0011] At the same time, due to the pressure relief effect of the Venturi mixer, the reaction products generated are flashed to form saturated steam and escape from the reaction tube, and the catalyst and solvent in the reaction tube return to the reactor.

[0012] Optionally, the raw materials for producing vinyl trichlorosilane are trichlorosilane and acetylene gas. The two raw materials are mixed in a raw material mixer and then enter the Venturi mixer. The diameter of the reaction tube is 80mm-150mm, and its length is 2000mm-3000mm. The flow rate of the gas-liquid two-phase mixture after decompression is 2m / s-3.5m / s.

[0013] Optionally, the method further comprises the following steps:

[0014] A portion of the solvent and catalyst mixture in the reactor is introduced into the reaction tower from the top in a spraying manner.

[0015] The gaseous material escaping from the reactor enters the reaction tower and contacts with the sprayed solvent and catalyst, so that the unreacted production raw materials in the gaseous material react under the action of the catalyst entering the reaction tower to generate reaction products. At the same time, the catalyst and solvent in the reaction tower are discharged into the reactor.

[0016] Optionally, the method further comprises the following steps:

[0017] The gaseous phase escaping from the reaction tower is introduced into a condenser for condensation to obtain a liquid crude vinyltrichlorosilane product.

[0018] Optionally, the reaction conditions provided by the reactor are: reaction temperature of 90-130° C.; reaction pressure of 0.05-0.1 MPa; the solvent is chlorobenzene or toluene, and the catalyst is a Karlsruhe catalyst.

[0019] Optionally, the method further comprises the following steps:

[0020] Part of the mixture of solvent and catalyst in the reactor is extracted, condensed and then fed back into the reactor to maintain the temperature of the reactor at 90-130°C.

[0021] Optionally, the reaction tube is provided with a stainless steel 316L wire mesh filler, and the reaction tower is provided with a ceramic filler.

[0022] Optionally, the method further comprises the following step: feeding the crude liquid vinyltrichlorosilane obtained by partial condensation into a reaction tower to maintain solvent balance.

[0023] The present invention also provides vinyltrichlorosilane produced by the above method.

[0024] The present invention also provides a vinyltrichlorosilane production system, comprising: a venturi mixer, a reaction kettle and a reaction tube.

[0025] The reactor is used to mix the solvent and the catalyst.

[0026] The venturi mixer is connected to the reactor and is used to input a portion of the solvent and catalyst mixture in the reactor into the generated vacuum, so that the raw materials for producing vinyltrichlorosilane are sucked into the venturi mixer and mixed with the solvent and catalyst entering the venturi mixer to form a gas-liquid two-phase mixture. The venturi mixer is also used to release the pressure of the gas-liquid two-phase mixture.

[0027] The upper part of the reaction tube is connected to a venturi mixer for receiving the depressurized gas-liquid two-phase mixture.

[0028] The lower part of the reaction tube extends into the reactor, and the reactor is also used to provide reaction conditions so that the production raw materials in the gas-liquid two-phase mixture react in the reaction tube under the action of the catalyst, and the generated reaction products are flash evaporated to form saturated steam under the pressure relief action of the venturi mixer and escape from the reaction tube, while the catalyst and solvent in the reaction tube return to the reactor.

[0029] Optionally, a reaction tower is further included, the reaction tower is connected to the reaction kettle, and a portion of the solvent and catalyst mixture in the reaction kettle enters the reaction tower from the top in a spraying manner.

[0030] The gaseous material escaping from the reactor enters the reaction tower and contacts with the sprayed solvent and catalyst, so that the unreacted production raw materials in the gaseous material react under the action of the catalyst entering the reaction tower to generate reaction products. At the same time, the catalyst and solvent in the reaction tower are discharged into the reactor.

[0031] Optionally, a condenser is further included, which is connected to the reaction tower and is used to condense the gaseous phase escaping from the reaction tower to obtain liquid crude vinyltrichlorosilane.

[0032] Optionally, a circulation pump is also included.

[0033] A liquid outlet pipe is provided at the bottom of the reactor, and the liquid outlet pipe is connected to the reaction tower and the venturi mixer respectively. The circulation pump is provided on the liquid outlet pipe and is used to circulate the solvent and the catalyst between the reactor and the venturi mixer, and between the reactor and the reaction tower.

[0034] Optionally, a heating jacket and a circulating cooler are also included.

[0035] The heating jacket is arranged on the outer wall of the reaction kettle and is used to heat the reaction kettle.

[0036] The circulation pump is connected to the top of the reactor and is used to circulate the solvent and catalyst between the bottom and the top of the reactor. The circulation cooler is arranged on the pipeline connecting the circulation pump and the top of the reactor and is used to cool the solvent and catalyst entering the top of the reactor so that the reactor maintains a stable reaction temperature.

[0037] Optionally, a reflux pipe is provided between the condenser and the reaction tower for feeding the partially condensed crude liquid vinyltrichlorosilane into the reaction tower to maintain solvent balance.

[0038] In the present invention, vinyl trichlorosilane raw materials (trichlorosilane and acetylene gas) and the mixed catalyst and solvent in the reactor are introduced into a venturi mixer to achieve efficient mixing of gas-liquid two-phases. The formed gas-liquid two-phase mixture is depressurized by the venturi mixer and enters a reaction tube placed in the reactor. Under the reaction conditions provided by the reactor, the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst. The generated reaction product is a light component, which is flash evaporated under the depressurization of the venturi mixer to form saturated steam and escape from the reaction tube, thereby avoiding the side reaction between the reaction product and the raw material trichlorosilane under the temperature provided by the reactor and the action of the catalyst, thereby greatly reducing the generation of the by-product 1,2-bis(trichlorosilyl)ethane. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 This is a schematic diagram of a vinyltrichlorosilane production system provided in Example 1 of the present invention.

[0040] In the figure: 1-trichlorosilane pipeline, 2-acetylene pipeline, 3-raw material mixer, 4-heating jacket, 5-Venturi mixer, 6-reaction tube, 7-reactor, 8-solvent pipeline, 9-steam pipeline, 10-condensate pipeline, 11-catalyst addition port, 12-reaction tower, 13-tower top gas phase pipeline, 14-condenser, 15-reaction tail gas vent pipe, 16-condensate feed pipe, 17-reflux pipe, 18-condensate extraction pipe, 19-circulating cooler, 20-circulating pump, 21-Venturi circulation pipeline, 22-reactor discharge pipe. DETAILED DESCRIPTION

[0041] The following will be combined with the accompanying drawings in the present invention to clearly and completely describe the technical solutions in the invention. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of the present invention.

[0042] In the description of the present invention, it should be noted that the directions or positional relationships indicated by “upper” and the like are based on the directions or positional relationships shown in the accompanying drawings and are only for the convenience and simplification of the description. They do not indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction. Therefore, they cannot be understood as limitations on the present invention.

[0043] In the description of the present invention, the terms “first” and “second” are used for descriptive purposes only and should not be understood as indicating or implying relative importance.

[0044] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connect", "set", "install", "fix" and the like should be understood in a broad sense, for example, it can be a fixed connection or a detachable connection, or an integral connection; it can be a direct connection or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0045] The present invention provides a method for producing vinyltrichlorosilane, comprising:

[0046] A portion of the solvent and catalyst mixture in the reaction kettle is introduced into a venturi mixer to generate a vacuum in the venturi mixer and a raw material for producing vinyltrichlorosilane is introduced into the venturi mixer to mix with the solvent and catalyst entering the venturi mixer to form a gas-liquid two-phase mixture,

[0047] The gas-liquid two-phase mixture is discharged into a reaction tube located in the reaction kettle and connected to the Venturi mixer during the pressure relief process of the Venturi mixer.

[0048] Under the reaction conditions provided by the reactor, the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst to generate a reaction product, vinyltrichlorosilane.

[0049] At the same time, due to the pressure relief effect of the Venturi mixer, the reaction products generated are flashed to form saturated steam and escape from the reaction tube, and the catalyst and solvent in the reaction tube return to the reactor.

[0050] The present invention also provides vinyltrichlorosilane produced by the above method.

[0051] The present invention also provides a vinyltrichlorosilane production system, comprising: a venturi mixer, a reaction kettle and a reaction tube.

[0052] The reactor is used to mix the solvent and the catalyst.

[0053] The venturi mixer is connected to the reactor and is used to input a portion of the solvent and catalyst mixture in the reactor into the generated vacuum, so that the raw materials for producing vinyltrichlorosilane are sucked into the venturi mixer and mixed with the solvent and catalyst entering the venturi mixer to form a gas-liquid two-phase mixture. The venturi mixer is also used to release the pressure of the gas-liquid two-phase mixture.

[0054] The upper part of the reaction tube is connected to a venturi mixer for receiving the depressurized gas-liquid two-phase mixture.

[0055] The lower part of the reaction tube extends into the reactor, and the reactor is also used to provide reaction conditions so that the production raw materials in the gas-liquid two-phase mixture react in the reaction tube under the action of the catalyst, and the generated reaction products are flash evaporated to form saturated steam under the pressure relief action of the venturi mixer and escape from the reaction tube, while the catalyst and solvent in the reaction tube return to the reactor.

[0056] Embodiment 1:

[0057] This embodiment provides a method for producing vinyltrichlorosilane, comprising:

[0058] A portion of the solvent and catalyst mixture in the reaction kettle 7 is introduced into a venturi mixer 5 to generate a vacuum in the venturi mixer 5 and a raw material for producing vinyltrichlorosilane is introduced into the venturi mixer 5 to mix with the solvent and catalyst entering the venturi mixer 5 to form a gas-liquid two-phase mixture.

[0059] The gas-liquid two-phase mixture is discharged into a reaction tube 6 located in a reaction kettle 7 and connected to the Venturi mixer 5 during the pressure relief process of the Venturi mixer 5.

[0060] Under the reaction conditions provided by the reactor 7, the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst to generate a reaction product, vinyltrichlorosilane.

[0061] At the same time, due to the pressure relief effect of the venturi mixer 5 , the reaction product generated is flashed to form saturated steam and escapes out of the reaction tube 6 , and the catalyst and solvent in the reaction tube 6 return to the reactor 7 .

[0062] The main reactions for the synthesis of vinyltrichlorosilane are as follows:

[0063] The main reaction chemical equation is as follows:

[0064] HSiCl3+C2H2——C2H3SiCl3 (exothermic reaction)

[0065] The main side reaction chemical equations are as follows:

[0066] HSiCl3+C2H3SiCl3——Cl3SiC2H4SiCl3

[0067] When carrying out the addition process, it is necessary to choose favorable production conditions as much as possible to reduce the occurrence of side reactions in order to increase the yield of vinyltrichlorosilane.

[0068] In this embodiment, the vinyl trichlorosilane raw material (trichlorosilane and acetylene gas) and the mixed catalyst and solvent in the reactor are introduced into the venturi mixer 5 to achieve efficient mixing of the gas-liquid two-phase. The formed gas-liquid two-phase mixture enters the reaction tube placed in the reactor after the pressure is released by the venturi mixer 5. Under the reaction conditions provided by the reactor 7, the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst, and the generated reaction product is a light component, which is flash evaporated under the pressure release of the venturi mixer 5 to form saturated steam and escape from the reaction tube 6, thereby avoiding the side reaction between the reaction product and the raw material trichlorosilane under the temperature provided by the reactor 7 and the action of the catalyst, thereby greatly reducing the generation of the by-product 1,2-bis(trichlorosilyl)ethane.

[0069] In this embodiment, the raw materials used to produce vinyl trichlorosilane are trichlorosilane and acetylene gas. The two raw materials are mixed in the raw material mixer 3 and then enter the venturi mixer 5. The diameter of the reaction tube 6 is 80mm-150mm, and its length is 2000mm-3000mm. The flow rate of the gas-liquid two-phase mixture after decompression is 2m / s-3.5m / s.

[0070] The production method of vinyltrichlorosilane mentioned in the background technology of this application still has the following technical problems: uneven mixing and distribution of raw materials, short reaction residence time, low raw material utilization rate, and insufficient reaction contact.

[0071] In this embodiment, the raw materials for producing vinyl trichlorosilane (trichlorosilane and acetylene gas) are fully mixed through the raw material mixer 3, the solvent and the catalyst are fully mixed through the reactor 7, and then the mixed raw materials in the raw material mixer 3 and a part of the mixed solvent and catalyst in the reactor 7 are introduced into the venturi mixer 5 for mixing. Another function of the venturi mixer 5 in this embodiment is to improve the mixing efficiency of the gas-liquid two phases, thereby solving the technical problems of uneven raw material mixing distribution and insufficient contact between the raw material and the catalyst in the prior art.

[0072] In addition, in this embodiment, by limiting the structure of the reaction tube 6 and the flow rate of the gas-liquid two-phase mixture after depressurization, practice shows that the reaction time can be controlled within 3-5s, so that more than 95% of the raw material trichlorosilane can be completely reacted, thereby ensuring full contact between the raw material and the catalyst and improving the raw material utilization rate.

[0073] The flow rate of the gas-liquid two-phase mixture after depressurization can be achieved by the pumping speed of the solvent and the catalyst, and the structural selection of the venturi mixer 5, which will not be described in detail here.

[0074] In this embodiment, the following steps are also included:

[0075] A portion of the mixture of solvent and catalyst in the reactor 7 is introduced into the reaction tower 12 from the top in a spraying manner.

[0076] The gaseous material escaping from the reactor 7 enters the reaction tower 12 and contacts with the solvent and catalyst sprayed down, so that the unreacted production raw materials in the gaseous material react under the action of the catalyst entering the reaction tower 12 to generate reaction products. At the same time, the catalyst and solvent in the reaction tower 12 are discharged into the reactor 7.

[0077] Thus, the raw materials that have not reacted fully can react in the reaction tower 12, and the reaction tower 12 also plays the role of a distillation tower to perform preliminary separation on the reaction mixed gas, reduce the amount of chlorobenzene added, and increase the content of the target product in the reaction condensate.

[0078] In this embodiment, the following steps are also included:

[0079] The gaseous phase escaping from the reaction tower 12 is introduced into the condenser 14 for condensation, and the reaction products and solvent in the gaseous phase are liquefied and separated from the unreacted acetylene gas, thereby obtaining a crude liquid vinyltrichlorosilane.

[0080] In this embodiment, the reaction conditions provided by the reactor 7 are: reaction temperature is 90-130° C.; reaction pressure is 0.05-0.1 MPa; solvent is chlorobenzene or toluene, and catalyst is Karlsruh catalyst.

[0081] In addition, the reaction temperature provided by the reactor 7 also ensures that the reaction product maintains a saturated steam state in the reactor 7 .

[0082] In this embodiment, the following steps are also included:

[0083] Part of the mixture of the solvent and the catalyst in the reaction kettle 7 is extracted, condensed, and then fed back into the reaction kettle 7, so that the temperature of the reaction kettle 7 is maintained at 90-130°C.

[0084] In this embodiment, a stainless steel 316L wire mesh filler is provided in the reaction tube 6, which is used to cut the mixed trichlorosilane and acetylene raw material gas to form small bubbles, increase the specific surface area, and fully combine with the chlorobenzene containing the catalyst, so that the reaction area is greatly increased, the reaction efficiency is greatly improved, and the utilization rate of the reaction raw material trichlorosilane is increased to more than 95%. At the same time, the dispersion effect of the filler is used to reduce the phenomenon of the reaction product and the reaction raw material trichlorosilane contacting again to generate secondary addition by-products. In the test and production process, fillers such as corrugated plates are selected, but the product yield after the reaction is low, the by-products are high, and the efficiency is low.

[0085] In this embodiment, the reaction tower 12 is provided with a corrugated ceramic filler for allowing the unreacted trichlorosilane to continue to react fully in the reaction tower, thereby reducing production costs. At the same time, the principle of the distillation tower is utilized to enable the reaction product vinyltrichlorosilane to be initially separated, and chlorobenzene is continuously returned to the reactor to ensure that the catalyst concentration in the reactor is relatively stable. The advantage of the small pressure difference of the corrugated filler is mainly utilized to enable the product vinyltrichlorosilane to be quickly separated.

[0086] In this embodiment, the crude liquid vinyltrichlorosilane (containing solvent) obtained by partial condensation is fed into the reaction tower 12 to maintain the solvent balance.

[0087] Embodiment 2:

[0088] This embodiment provides vinyltrichlorosilane produced by the method of the embodiment.

[0089] Embodiment 3:

[0090] This embodiment provides a vinyl trichlorosilane production system, such as Figure 1 As shown, it includes: a venturi mixer 5, a reaction kettle 7 and a reaction tube 6,

[0091] Reactor 7 is used to mix the solvent and the catalyst.

[0092] The venturi mixer 5 is connected to the reactor 7 and is used to input a portion of the solvent and catalyst mixture in the reactor 7 into the generated vacuum, so that the raw materials for producing vinyltrichlorosilane are sucked into the venturi mixer 5 and mixed with the solvent and catalyst entering the venturi mixer 5 to form a gas-liquid two-phase mixture. The venturi mixer 5 is also used to release the pressure of the gas-liquid two-phase mixture.

[0093] The upper part of the reaction tube 6 is connected to the venturi mixer 5 for receiving the depressurized gas-liquid two-phase mixture.

[0094] The lower part of the reaction tube 6 extends into the reactor 7, and the reactor 7 is also used to provide reaction conditions so that the production raw materials in the gas-liquid two-phase mixture react in the reaction tube 6 under the action of the catalyst, and the generated reaction products are flashed under the pressure relief action of the venturi mixer 5 to form saturated steam to escape from the reaction tube 6, and at the same time, the catalyst and solvent in the reaction tube 6 return to the reactor 7.

[0095] Thus, the vinyl trichlorosilane raw material (trichlorosilane and acetylene gas) and the mixed catalyst and solvent in the reactor are introduced into the venturi mixer 5 to achieve efficient mixing of the gas-liquid two-phase. The formed gas-liquid two-phase mixture enters the reaction tube placed in the reactor after the pressure is released by the venturi mixer 5. Under the reaction conditions provided by the reactor 7, the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst, and the generated reaction product is a light component, which is flash evaporated under the pressure release of the venturi mixer 5 to form saturated steam and escape from the reaction tube 6, thereby avoiding the side reaction between the reaction product and the raw material trichlorosilane under the temperature provided by the reactor 7 and the action of the catalyst, thereby greatly reducing the generation of the by-product 1,2-bis(trichlorosilyl)ethane.

[0096] In this embodiment, before the raw materials, solvent and catalyst are introduced into the venturi mixer, the following steps are also included:

[0097] The raw materials for producing vinyltrichlorosilane are introduced into a raw material mixer 3 for mixing.

[0098] The solvent and the catalyst are introduced into a reaction vessel 7 for mixing.

[0099] The raw materials (trichlorosilane and acetylene gas) for producing vinyl trichlorosilane are fully mixed through the raw material mixer 3, the solvent and the catalyst are fully mixed through the reactor 7, and then the mixed raw materials in the raw material mixer 3 and a part of the mixed solvent and catalyst in the reactor 7 are introduced into the venturi mixer 5 for mixing. Another function of the venturi mixer 5 in this embodiment is to improve the mixing efficiency of the gas-liquid two phases, thereby solving the technical problems of uneven raw material mixing distribution and insufficient contact between the raw material and the catalyst in the prior art.

[0100] In this embodiment, a reaction tower 12 is also included. The reaction tower 12 is connected to the reaction kettle 7. A portion of the solvent and catalyst mixture in the reaction kettle 7 enters the reaction tower 12 from the top in a spraying manner.

[0101] The gaseous material escaping from the reactor 7 enters the reaction tower 12 and contacts with the solvent and catalyst sprayed down, so that the unreacted production raw materials in the gaseous material react under the action of the catalyst entering the reaction tower 12 to generate reaction products. At the same time, the catalyst and solvent in the reaction tower 12 are discharged into the reactor 7.

[0102] Thus, the raw materials that have not reacted fully can react in the reaction tower 12, and the reaction tower 12 also plays the role of a distillation tower to perform preliminary separation on the reaction mixed gas, reduce the amount of chlorobenzene added, and increase the content of the target product in the reaction condensate.

[0103] In this embodiment, a condenser 14 is further included. The condenser 14 is connected to the reaction tower 12 and is used to condense the gaseous phase escaping from the reaction tower 12. The reaction products and solvents in the gaseous phase are liquefied and separated from the unreacted acetylene gas to obtain liquid crude vinyltrichlorosilane.

[0104] In this embodiment, a circulation pump 20 is also included.

[0105] A liquid outlet pipe is provided at the bottom of the reactor 7, and the liquid outlet pipe is connected to the reaction tower 12 and the venturi mixer 5 respectively. A circulation pump 20 is provided on the liquid outlet pipe for circulating the solvent and the catalyst between the reactor 7 and the venturi mixer 5, and between the reactor 7 and the reaction tower 12. The flow rate of the solvent and catalyst mixed liquid entering the venturi mixer 5 can be controlled by controlling the rotation speed of the circulation pump 20.

[0106] In this embodiment, a heating jacket 4 and a circulating cooler 19 are also included.

[0107] The heating jacket 4 is arranged on the outer wall of the reaction kettle 7 and is used to heat the reaction kettle 7.

[0108] The circulation pump 20 is connected to the top of the reactor 7, and is used to circulate the solvent and the catalyst between the bottom and the top of the reactor 7. The circulation cooler 19 is arranged on the pipeline connecting the circulation pump 20 and the top of the reactor 7, and is used to cool the solvent and the catalyst entering the top of the reactor 7, so that the reactor 7 maintains a stable reaction temperature.

[0109] In this embodiment, a reflux pipe 17 is provided between the condenser 14 and the reaction tower 12 for feeding the partially condensed crude liquid vinyltrichlorosilane into the reaction tower 12 to maintain solvent balance.

[0110] In summary, in this embodiment, the raw material mixer 3, the venturi mixer 5, the reaction tube 6, the reactor 7 and the reaction tower 12 are combined. The raw material trichlorosilane and acetylene gas are first fully mixed through the raw material mixer 3, and then enter the venturi mixer 5 after mixing to fully contact the circulating liquid (solvent and catalyst) introduced from the reactor, and then react in the reaction tube 6. The unreacted raw material is further reacted in the reaction tower 12. After cooling, a part of the gas phase material at the top of the tower returns to the reaction tower 12 to maintain balance, and a part is extracted to the crude product buffer tank to wait for distillation. The liquid after the reaction is completed is discharged through the low discharge port of the kettle, and the condensate at the top of the tower is sent to the crude product buffer tank to wait for distillation. During the period, when the temperature is low, it is heated by the heating jacket 4 of the reactor 7, and when the temperature is high, it is cooled by the circulating cooler 19 to keep the temperature of the reaction system stable. Compared with the existing vinyl trichlorosilane synthesis scheme, the scheme of this embodiment can effectively solve the problems of poor mixing uniformity of reaction raw materials, short reaction contact time, low utilization rate of reaction raw materials, high catalyst unit consumption, etc., and provide a basis for large-scale production.

[0111] The working principle of the synthesis method and system provided in this embodiment is as follows: first, a certain amount of solvent and corresponding catalyst are added to the reactor 7, and the circulation pump 20 of the reactor 7 is turned on. A part of the solvent enters the venturi mixer 5, and the rest is used as the eluent of the reaction tower 12 and the reactor 7 to balance the temperature.

[0112] The circulating liquid entering the venturi mixer 5 has a certain pressure, and it is ejected at a high speed through the nozzle of the venturi mixer 5, so that the pressure energy is converted into speed energy (pressure relief produces a large number of bubbles), and a vacuum is formed in the suction chamber of the venturi mixer 5, so that the acetylene and trichlorosilane mixed gas mixed by the raw material mixer 3 is sucked into the venturi mixer 5, and mixed with the circulating liquid with a large number of bubbles, so as to achieve efficient contact and mixing of gas and liquid phases. The formed gas-liquid two-phase mixture is discharged into the reaction tube 6, and the reaction tube 6 is provided with a wire mesh mixer, and fully contacts with the catalyst in the circulating liquid in the reaction tube 6, and contacts for a sufficient time in the reaction tube 6 to ensure the reaction contact time. The unreacted raw materials pass through the reaction tower 12, and further react under the action of the eluent, thereby improving the utilization rate of the raw materials and effectively reducing the unit consumption of catalysts and by-products.

[0113] The specific production process of vinyl trichlorosilane in this embodiment is as follows:

[0114] Solvent is added to the reactor 7 through the solvent pipeline 8. The volume of the reactor 7 is preferably 3-5 cubic meters, and the material is preferably enamel equipment. The amount of solvent added is 1 / 2 to 2 / 3 of the volume of the reactor. Chlorobenzene or toluene is preferably selected as the solvent, and the catalyst is added to the reactor 7 through the catalyst addition port 11 at the upper end of the reactor 7. The catalyst for the formation of vinyl trichlorosilane is mainly based on the Group VIII metal, and chloroplatinic acid is preferably selected as the main catalyst, and isopropyl alcohol and triphenylphosphine are selected as ligands. Each reactor is preferably added in an amount of 20 to 50 g. In this embodiment, the catalyst is selected from the Karlster catalyst.

[0115] After adding the solvent and the catalyst, the reactor circulation pump 20 is turned on to start circulating to fully mix the catalyst and the solvent. By adjusting the outlet of the circulation pump 20, the circulation volume entering the venturi mixer 5 is controlled to be 6-8 cubic meters / hour, the circulation volume entering the reaction tower 12 is controlled to be 2-5 cubic meters / hour, and the reactor cooling circulation volume is controlled to be 1-3 cubic meters / hour.

[0116] The reactor 7 is provided with a heating jacket 4, and steam is introduced into the heating jacket 4 through a steam pipeline 9 to slowly heat the reactor 7. The reactor is provided with temperature, pressure and other monitoring elements to raise the temperature to 90-130°C, and the pressure is preferably selected to be 0.05-0.1MPa. The generated steam condensate is discharged from the system through a condensate pipeline 10 and sent to a collection tank for use by the power plant. The reactor 7 reaches the catalyst reaction temperature to ensure the activity of the catalyst. At the same time, the circulating cooler 19 is opened for cooling circulation to keep the temperature fluctuation range within ±5°C.

[0117] The vaporized raw trichlorosilane is introduced into the raw material mixer 3 through the trichlorosilane pipeline 1, and the acetylene gas is introduced into the raw material mixer 3 through the acetylene pipeline 2, and the trichlorosilane and acetylene gases are combined in a certain ratio. The acetylene feed rate is controlled at 30-40 kg / hour. When entering the gas phase inlet of the venturi mixer 5, the pressure of trichlorosilane and acetylene is preferably selected to be 0.1-0.2 MPa, the molar ratio of trichlorosilane and acetylene is 1:2.5-3.5, and the temperature of the gas after mixing is 100-120°C. The diameter of the raw material mixer 3 is preferably DN40-DN80. The venturi mixer 5 uses the venturi principle. Under the impetus of the circulating liquid entering through the venturi circulation pipeline 21, the venturi forms a slightly negative pressure state, thereby reducing the resistance of the raw material gas to enter. The raw material mixed gas is contacted and mixed with the circulating liquid containing the catalyst in the venturi mixer 5. In the reaction Further mixing and contacting are carried out in tube 6, and a reaction occurs. The reaction time in the reaction tube is preferably 3-5 seconds, the reaction tube is DN80-DN150, the reaction tube length is preferably 2400mm, the reaction tube temperature is 90-130°C, which is consistent with the reactor, and the reactor pressure is 0.05-0.1MPa. Since the reaction is an exothermic reaction, it is necessary to adjust the opening of the cooling water of the circulating cooler 19 to remove the reaction heat from the system in time to avoid overheating of the reactor. At the same time, the reaction tube 6 is inserted into the bottom of the reactor 7, and the generated mixed gas is vaporized in the reactor 7 and enters the reaction tower 12 with the unreacted raw material mixed gas.

[0118] The unreacted raw material mixed gas in the reaction tower 12 contacts the reaction tower eluent containing the catalyst which is depressurized through the Venturi circulation pipeline 21 again, and continues to react, so as to ensure the full reaction of the raw materials and reduce the waste of the reaction raw materials. The material of the reaction tower 12 is preferably enamel equipment, the filler is ceramic filler, the filler model is preferably 350Y, the tower diameter is 500-800mm, the tower height is 8-12 meters, and the pressure is 0.05-0.1MPa, which is consistent with the reactor pressure.

[0119] The gaseous phase rising from the reaction tower 12 enters the condenser 14 through the tower top gas phase pipeline 13 for cooling, and the resulting reaction mixture is collected through the condensate discharge pipe 16.

[0120] A part of it is returned to the reaction tower 12 through the reflux pipe 17 to ensure the solvent balance of the reaction tower, and the other part is sent to the crude product buffer tank through the condensate extraction pipe 18 to be distilled. The unreacted acetylene and other non-condensable gases are discharged through the reaction tail gas vent pipe 15. Since part of the solvent in the reactor 7 is carried out of the system with the product, it is necessary to regularly add solvent chlorobenzene or toluene to the reactor 7 through the solvent pipeline 8 to maintain the liquid level balance.

[0121] According to the sampling and analysis data, when the by-products in the reactor 7 reach 2%-10%, the reactor feed is stopped, the reactor is cooled to below 60°C by circulation, and the reactor materials are mixed with the condensate at the top of the reaction tower through the reactor discharge pipe 22 and sent to the buffer tank for distillation.

[0122] It is to be understood that the above embodiments are merely exemplary embodiments used to illustrate the principles of the present invention, but the present invention is not limited thereto. For those of ordinary skill in the art, various modifications and improvements can be made without departing from the spirit and essence of the present invention, and these modifications and improvements are also considered to be within the scope of protection of the present invention.

Claims

1. A method for producing vinyltrichlorosilane, comprising: A portion of the solvent and catalyst mixture in the reaction kettle (7) is introduced into a venturi mixer (5) to generate a vacuum in the venturi mixer (5) and a raw material for producing vinyltrichlorosilane is introduced into the venturi mixer (5) to mix with the solvent and catalyst entering the venturi mixer (5) to form a gas-liquid two-phase mixture. The gas-liquid two-phase mixture is discharged into a reaction tube (6) located in a reaction kettle (7) and connected to the Venturi mixer (5) during the pressure relief process of the Venturi mixer (5). Under the reaction conditions provided by the reactor (7), the raw materials in the gas-liquid two-phase mixture react under the action of the catalyst to generate a reaction product, vinyltrichlorosilane. At the same time, due to the pressure relief effect of the venturi mixer (5), the reaction product generated is flashed to form saturated steam and escapes from the reaction tube (6), and the catalyst and solvent in the reaction tube (6) return to the reaction kettle (7); The raw materials for producing vinyl trichlorosilane are trichlorosilane and acetylene gas. The two raw materials are mixed in a raw material mixer (3) and then enter the venturi mixer (5). The reaction conditions provided by the reactor (7) are: a reaction temperature of 90-130° C.; a reaction pressure of 0.05-0.1 MPa; the solvent is chlorobenzene or toluene, and the catalyst is a Karlsruhe catalyst.

2. The method for producing vinyltrichlorosilane according to claim 1, characterized in that: The diameter of the reaction tube (6) is 80 mm to 150 mm, its length is 2000 mm to 3000 mm, and the flow rate of the gas-liquid two-phase mixture after depressurization is 2 m / s to 3.5 m / s.

3. The method for producing vinyltrichlorosilane according to claim 1, characterized in that: The following steps are also included: A portion of the mixture of solvent and catalyst in the reaction kettle (7) is introduced into the reaction tower (12) from the top in a spraying manner. The gaseous material escaping from the reaction kettle (7) enters the reaction tower (12) and contacts the solvent and catalyst sprayed down, so that the unreacted production raw materials in the gaseous material react under the action of the catalyst entering the reaction tower (12) to generate reaction products. At the same time, the catalyst and solvent in the reaction tower (12) are discharged into the reaction kettle (7).

4. The method for producing vinyltrichlorosilane according to claim 3, characterized in that: The following steps are also included: The gaseous phase escaping from the reaction tower (12) is introduced into the condenser (14) for condensation to obtain a liquid crude vinyltrichlorosilane.

5. The method for producing vinyltrichlorosilane according to any one of claims 1 to 4, characterized in that: The following steps are also included: Part of the mixture of the solvent and the catalyst in the reaction kettle (7) is extracted, condensed, and then fed back into the reaction kettle (7) so that the temperature of the reaction kettle (7) is maintained at 90-130°C.

6. The method for producing vinyltrichlorosilane according to claim 3 or 4, characterized in that: The reaction tube (6) is provided with a stainless steel 316L wire mesh filler, and the reaction tower (12) is provided with a corrugated ceramic filler.

7. The method for producing vinyltrichlorosilane according to claim 3 or 4, characterized in that: The method further comprises the following steps: feeding the partially condensed crude liquid vinyltrichlorosilane into a reaction tower (12) to maintain solvent balance.

8. A vinyltrichlorosilane production system, characterized in that: include: Venturi mixer (5), reactor (7) and reaction tube (6), The reaction kettle (7) is used to mix the solvent and the catalyst. The venturi mixer (5) is connected to the reactor (7) and is used to input a portion of the solvent and catalyst mixture in the reactor (7) into the generated vacuum, so that the raw material for producing vinyltrichlorosilane is sucked into the venturi mixer (5) and mixed with the solvent and catalyst entering the venturi mixer (5) to form a gas-liquid two-phase mixture. The venturi mixer (5) is also used to release the pressure of the gas-liquid two-phase mixture. The upper part of the reaction tube (6) is connected to the Venturi mixer (5) for receiving the depressurized gas-liquid two-phase mixture. The lower part of the reaction tube (6) extends into the reaction kettle (7), and the reaction kettle (7) is also used to provide reaction conditions so that the production raw materials in the gas-liquid two-phase mixture react in the reaction tube (6) under the action of the catalyst, and the generated reaction products are flash evaporated under the pressure relief action of the venturi mixer (5) to form saturated steam and escape from the reaction tube (6), while the catalyst and solvent in the reaction tube (6) return to the reaction kettle (7); The raw materials for producing vinyl trichlorosilane are trichlorosilane and acetylene gas. The two raw materials are mixed in a raw material mixer (3) and then enter the venturi mixer (5). The reaction conditions provided by the reactor (7) are: a reaction temperature of 90-130° C.; a reaction pressure of 0.05-0.1 MPa; the solvent is chlorobenzene or toluene, and the catalyst is a Karlsruhe catalyst.

9. The vinyltrichlorosilane production system according to claim 8, characterized in that: The reactor also comprises a reaction tower (12), wherein the reaction tower (12) is connected to the reactor (7), and a portion of the solvent and catalyst mixture in the reactor (7) enters the reaction tower (12) from the top in a spraying manner. The gaseous material escaping from the reaction kettle (7) enters the reaction tower (12) and contacts the solvent and catalyst sprayed down, so that the unreacted production raw materials in the gaseous material react under the action of the catalyst entering the reaction tower (12) to generate reaction products. At the same time, the catalyst and solvent in the reaction tower (12) are discharged into the reaction kettle (7).

10. The vinyltrichlorosilane production system according to claim 9, characterized in that: The invention also comprises a condenser (14), which is connected to the reaction tower (12) and is used to condense the gaseous phase escaping from the reaction tower (12) to obtain a liquid crude vinyltrichlorosilane product.

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