CN211411975U - Vinyl trichlorosilane synthesizer - Google Patents
Vinyl trichlorosilane synthesizer Download PDFInfo
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- CN211411975U CN211411975U CN201921945730.3U CN201921945730U CN211411975U CN 211411975 U CN211411975 U CN 211411975U CN 201921945730 U CN201921945730 U CN 201921945730U CN 211411975 U CN211411975 U CN 211411975U
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Abstract
The utility model provides a vinyl trichlorosilane synthesizer, which comprises a vaporizer and a reactor; the vaporizer is communicated with the reactor through a gas guide pipe; the vaporizer includes a first heating unit and a vaporizer main body; the first heating unit heats the vaporizer main body; the vaporizer main body is provided with an acetylene gas inlet and a trichlorosilane inlet and is used for conveying the mixed gas of trichlorosilane and acetylene added into the vaporizer main body into the reactor through a gas guide pipe; the reactor comprises a temperature control unit, a condenser and a reactor main body; the gas-guide tube extends into the lower part of the reactor main body; the temperature control unit is arranged at the lower part of the reactor main body and is used for controlling the temperature of the lower part of the reactor main body; the condenser is arranged on the upper part of the reactor main body and is used for condensing the gas in the reactor main body. The utility model discloses a synthesizer can simulate vinyl trichlorosilane's synthesis in the laboratory, carries out process optimization, and the experiment is verified, establishes good technology experimental study basis for industrial production.
Description
Technical Field
The utility model belongs to the technical field of the synthesis of silane new material, concretely relates to vinyl trichlorosilane synthesizer.
Background
The vinyl trichlorosilane is an important chemical product, and is an important raw material for synthesizing various other vinyl organosilicon coupling agents.
In the field of synthesis, laboratory stages are generally needed for further application to actual production. The laboratory stage is an important stage, various problems in the process can be found at an early stage, industrial production process parameters are simulated, and optimization and solution are carried out at an early stage, so that the cost is saved. However, laboratory equipment in the prior art is a conventional simple laboratory vessel, lacks an experimental device specially for synthesizing vinyltrichlorosilane, cannot well simulate industrial production process conditions of vinyltrichlorosilane, and cannot meet experimental requirements.
SUMMERY OF THE UTILITY MODEL
The utility model discloses in order to solve at least partially that the laboratory paraphernalia that exists is simple, the technical problem of simulation vinyl trichlorosilane industrial production process condition that can't be fine and accomplished the utility model discloses.
Solve the utility model discloses the technical scheme that technical problem adopted is:
the utility model provides a vinyl trichlorosilane synthesizer, which comprises a vaporizer and a reactor; the vaporizer is communicated with the reactor through a gas guide pipe;
the vaporizer includes a first heating unit and a vaporizer main body; the first heating unit is used for heating the interior of the vaporizer main body; the vaporizer main body is provided with an acetylene gas inlet and a trichlorosilane inlet and is used for conveying mixed gas of trichlorosilane and acetylene which is added into the vaporizer main body and heated and vaporized by the first heating unit into the reactor through a gas guide pipe;
the reactor comprises a temperature control unit, a condenser and a reactor main body; the gas guide pipe extends into the lower part of the reactor main body; the temperature control unit is arranged at the lower part of the reactor main body and is used for controlling the temperature of the lower part of the reactor main body so as to keep the temperature within a preset temperature range; the condenser is arranged at the upper part of the reactor main body and is used for condensing the gas at the upper part of the reactor main body.
Further, the vaporizer main body is a first multi-mouth flask; the first heating unit is a heating sleeve and is arranged at the bottom of the first multi-mouth flask; the vaporizer also comprises a first temperature measuring instrument which is used for measuring the internal temperature of the first multi-mouth flask;
the reactor main body comprises a second multi-mouth flask and a glass cylinder, and the glass cylinder is arranged at the lower part of the second multi-mouth flask and communicated with the second multi-mouth flask; the temperature control unit comprises a heater, a second temperature measuring instrument and a cooler, wherein the heater is used for heating the reactant in the glass cylinder, the second temperature measuring instrument is used for measuring the temperature of the reactant in the glass cylinder, and the cooler is used for cooling the reactant in the glass cylinder when the temperature of the reactant is higher than a preset temperature value; the condenser is arranged at the upper part of the second multi-mouth flask and is communicated with the second multi-mouth flask.
Further, the air duct extends into the bottom of the glass cylinder; the lower end of the gas guide pipe is provided with a gas distributor.
Further, the heater is an electric heating belt wound outside the glass cylinder.
Further, the cooler is a glass coil embedded in the glass cylinder, and cooling water is introduced into the glass coil to cool the glass cylinder.
Further, the measuring end of the first thermometer extends into the first multi-mouth flask from the upper part of the first multi-mouth flask; and the measuring end of the second thermometer extends into the bottom of the second multi-mouth flask from the upper part of the second multi-mouth flask and continues to extend into the glass cylinder.
Furthermore, the bottom of the glass cylinder body is provided with a discharge valve and a discharge hole.
Furthermore, a cooling water pipe is wound outside the condenser, and cooling water is introduced into the cooling water pipe.
Further, an acetylene gas inlet pipe is arranged at the acetylene gas inlet; and a gas glass rotameter is arranged on the acetylene gas inlet pipe and used for controlling the gas inlet flow of acetylene.
Further, a dropping funnel is arranged at the trichlorosilane inlet; the dropping funnel is a constant pressure dropping funnel.
Has the advantages that:
vinyl trichlorosilane synthesizer, have the reaction heating and heat up, the exothermic function of cooling accuse temperature of reaction, the vaporizer has the function that makes liquid raw material trichlorosilane vaporization to it is the bubbling in the gaseous form gets into the reactor with acetylene mixture, the reaction is more abundant. The gas glass rotameter can accurately measure the air input of acetylene and ensure the accurate proportioning of materials. The gas distributor on the gas-guide tube can ensure that the mixed gas of trichlorosilane and acetylene which are raw materials for reaction is uniformly distributed in the reaction solvent. The glass cylinder increases the retention time of the mixed gas of acetylene and trichlorosilane in the reaction solvent, and the two raw materials can be fully reacted. The device can simulate the synthesis of the vinyl trichlorosilane in a laboratory, can perform process optimization and experimental verification, and lays a good process technology experimental research foundation for industrial production. Has the advantages of good effect, high product yield and reliable use.
Drawings
FIG. 1 is a schematic structural diagram of a vinyltrichlorosilane synthesizing apparatus according to an embodiment of the present invention;
in the figure: 1-gas guide tube; 2-a first heating unit; 3-a vaporizer body; a 4-acetylene gas inlet; 5-trichlorosilane entrance; 6-a temperature control unit; 61-a heater; 62-a second temperature measuring instrument; 63-a cooler; 7-a condenser; 8-a reactor body; 81-second multi-neck flask; 82-glass cylinder; 9-a first temperature measuring instrument; 10-a gas distributor; 11-a discharge valve; 12-discharging port; 13-acetylene inlet pipe; 14-gas glass rotameter; 15-constant pressure dropping funnel.
Detailed Description
In order to make the technical solution of the present invention better understood by those skilled in the art, the present invention will be described in further detail with reference to the accompanying drawings and examples.
It should be noted that, in the case of no conflict, the features in the embodiments of the present invention may be arbitrarily combined with each other.
In which the terminology used in the embodiments of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. As used in the embodiments of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
Vinyltrichlorosilane is an important chemical product, is mainly used for organic synthesis, and is used as an intermediate for silicone manufacture, a coupling agent of an adhesive and a chemical reagent. Meanwhile, the modified polyvinyl chloride is an important raw material for synthesizing various other vinyl organosilicon coupling agents, and is used for modifying chlorine-containing resins (such as polyvinyl chloride and the like) or copolymerizing chlorine-containing monomers. Vinyltrichlorosilane is also useful as a surface treatment for glass fibers and as a treatment for reinforced plastic laminates to improve the mechanical strength and heat and moisture resistance of the article.
The formula of the vinyltrichlorosilane is CH2＝CHSiCl3. The synthesis method mainly comprises a thermal condensation method and a thermal addition method; the thermal condensation method is to obtain vinyl trichlorosilane through condensation of chloroethylene and trichlorosilane, and the addition method is to add acetylene and trichlorosilane. Among them, the thermal addition method has good economic efficiency due to its low cost, and is widely used in industrial production, but in the process production, since the vinyl trichlorosilaneAnd trichlorosilane is easy to flow and volatilize, is extremely easy to burn in air, has the risk of catching fire at the temperature below 18 ℃ below zero, and can burn strongly when exposed to open fire, and trichlorosilane steam can form explosive mixed gas with wide concentration range with air to cause violent explosion when heated. The vinyl trichlorosilane is flammable and is flammable when meeting high heat, open fire or being contacted with an oxidant, toxic and corrosive, reacts violently during hydrolysis, has high requirements on various production environments of industrial production, and is easy to generate various problems. In addition, when the addition method is used for producing the vinyl trichlorosilane, a catalyst and a non-polar solvent are required, the variety of the catalyst and the solvent is various, and the production process parameters such as the proportion of acetylene to trichlorosilane and the reaction temperature have influence on the yield of the vinyl trichlorosilane. Therefore, the method is further applied to actual production after a laboratory stage so as to solve various problems in the actual production, simulate industrial production process parameters, optimize the solution in the early stage, save the cost and play an important role, but the prior art adopts an experimental device which is temporarily built through a conventional simple experimental utensil, so that the industrial production process conditions can not be well simulated, and a vinyl trichlorosilane synthesis device which can well simulate the actual production in a laboratory is lacked so as to meet the experimental needs. Therefore, the embodiment of the utility model provides a vinyl trichlorosilane synthesizer.
As shown in fig. 1, an embodiment of the present invention provides a vinyl trichlorosilane synthesis apparatus, including a vaporizer and a reactor; the vaporizer is communicated with the reactor through a gas guide tube 1;
the vaporizer includes a first heating unit 2 and a vaporizer main body 3; the first heating unit 2 is used for heating the inside of the vaporizer main body 3; the vaporizer main body 3 is provided with an acetylene gas inlet 4 and a trichlorosilane inlet 5 and is used for conveying mixed gas of trichlorosilane and acetylene which is added into the vaporizer main body and heated and vaporized by the first heating unit 2 into the reactor through a gas guide tube 1;
the reactor comprises a temperature control unit 6, a condenser 7 and a reactor body 8; the gas-guide tube 1 extends into the lower part of the reactor main body 8; the temperature control unit 6 is arranged at the lower part of the reactor main body 8 and is used for controlling the temperature of the lower part of the reactor main body 8 so as to keep the temperature within a preset temperature range; the condenser 7 is arranged at the upper part of the reactor main body 8 and is used for condensing gas at the upper part of the reactor main body 8, specifically, unreacted trichlorosilane and vaporized vinyl trichlorosilane.
Under a certain pressure, taking metal in a VIII family as a catalyst, reacting trichlorosilane with acetylene to generate vinyl trichlorosilane, and simultaneously generating 1, 2-bis (trichlorosilane-based) ethylene; the chemical reaction equation for synthesizing the vinyltrichlorosilane by the addition method is as follows:
HSiCl3+C2H2——C2H3SiCl3
the chemical equation for the main side reaction is as follows:
HSiCl3+C2H3SiCl3——Cl3SiC2H4SiCl3(10％)。
when the addition method is used for production, favorable production conditions are selected as much as possible, and the occurrence of side reactions is reduced, so that the yield of the vinyl trichlorosilane is improved.
The utility model discloses during synthesizer use, add chlorobenzene, catalyst in to the reactor main part 8 of reactor, the condensate water is led to condenser 7, and the trichlorosilane of measurement is added to vaporizer main part 3 to let in acetylene. The first heating unit 2 of the vaporizer, typically an electric heating jacket, is turned on, and the interior of the vaporizer is warmed to 50-60 ℃. Trichlorosilane dripped into the vaporizer main body 3 is vaporized and mixed with acetylene and then is introduced into the reactor through the gas guide tube 1 for reaction. The temperature of the solvent in the reactor body 8 was raised to 75-85 ℃ by the temperature control unit 6 of the reactor. The exothermic temperature rises during the reaction and unreacted trichlorosilane and vaporized vinyltrichlorosilane are condensed in a condenser 7.
Further, the vaporizer main body 3 is a first multi-neck flask, and the first heating unit 2 is a heating jacket and is arranged at the bottom of the first multi-neck flask; the vaporizer also comprises a first temperature measuring instrument 9 for measuring the internal temperature of the first multi-neck flask;
the reactor main body 8 comprises a second multi-mouth flask 81 and a glass cylinder 82, and the glass cylinder 82 is arranged at the lower part of the second multi-mouth flask 81 and communicated with the second multi-mouth flask 81; the temperature control unit 6 comprises a heater 61, a second temperature measuring instrument 62 and a cooler 63, wherein the heater 61 is used for heating the reactant in the glass cylinder 82, the second temperature measuring instrument 62 is used for measuring the temperature of the reactant in the glass cylinder 82, and the cooler 63 is used for cooling the reactant in the glass cylinder 82 when the temperature is higher than a preset temperature value; the condenser 7 is disposed on the upper portion of the second multi-neck flask 81 and is communicated with the second multi-neck flask 81.
The first multi-neck flask of this embodiment may be a conventional round-bottom three-neck flask, and the second multi-neck flask 81 may be a round-bottom three-neck flask having a bottom communicating with a glass cylinder 82. When the device is used, the metered trichlorosilane is added into the vaporizer, the acetylene is introduced into the vaporizer, and the mixture is filled into the reactor after being mixed. The temperature control unit 6 controls the power of the heater 61 according to the temperature inside the glass cylinder 82 measured by the second thermometer 62, and determines whether to turn on the cooler 63, so that the sealing performance of each device is ensured when in use, and gas leakage is not generated.
Further, the gas-guide tube 1 extends into the bottom of the glass cylinder 82; the lower end of the gas guide tube 1 is provided with a gas distributor 10.
The gas guide pipe 1 extends into the bottom of the glass cylinder 82, trichlorosilane is mixed with acetylene after being vaporized, and the mixture is uniformly bubbled in the reactor through the gas guide pipe 1 and the gas distributor 10 to react, so that the gas can be mixed more uniformly, and the contact area between the gas and a catalyst during the reaction is increased.
Further, the heater 61 is an electric heating tape wound on the outside of the glass cylinder 82.
When the additive method is used for production, the platinum black, the platinum rubber and the platinum asbestos are effective catalysts, when the reaction temperature is about 80 ℃, the catalysts have better activity and selectivity for the reaction, the temperature is too high, black precipitates are easy to appear in the catalysts in the reaction process, the catalysts gradually lose activity, the yield is reduced, the selectivity is low, the temperature is low, the activity of the catalysts is not exerted to the maximum, and the activity and the selectivity are also reduced. The solvent and the catalyst are mainly placed in the glass cylinder 82, the glass cylinder 82 can prolong the reaction time, so that the reaction is more sufficient, the electric heating belt wound outside the glass cylinder 82 can enable the temperature in the glass cylinder 82 to reach a proper temperature, the heating area is increased, and the temperature in the glass cylinder 82 during the reaction is more uniform.
Further, the cooler 63 is a glass coil embedded inside the glass cylinder 82, and cooling water is introduced into the glass coil to cool the glass cylinder 82.
The addition reaction is exothermic, the exothermic reaction temperature can exceed 90 ℃ and easily exceed the boiling point (90.6-104.8 ℃) of the vinyl trichlorosilane, so that the produced vinyl trichlorosilane is changed into steam, the water is introduced into a glass coil pipe to be cooled to 75-85 ℃, the vinyl trichlorosilane can be kept to be liquid, and the catalyst has better activity and selectivity.
Further, the measuring end of the first thermometer 9 extends into the first multi-neck flask from the upper part of the first multi-neck flask; the measuring end of the second thermometer 62 extends from the upper part of the second multi-neck flask 81 to the bottom of the second multi-neck flask 81 and continues to extend into the glass cylinder 82.
The first thermometer 9 and the second thermometer 62 can use thermometers, and the thermometers extend into the first multi-neck flask from the mouth of the first multi-neck flask; and a glass cylinder 82 extending from the mouth of the second multi-neck flask 81 to the bottom of the second multi-neck flask 81. The real-time temperature in the vaporizer and the reactor can be truly reflected through the two thermometers, the reaction is favorably controlled, and the influence of the real reaction temperature on the reaction is obtained.
Further, the bottom of the glass cylinder 82 of the reactor is provided with a discharge valve 11 and a discharge port 12.
After a certain reaction time or after the reaction of adding quantitative reactants is completed, the temperature is reduced, the discharge valve 11 is opened to discharge the reaction materials from the discharge port 12, and the obtained reaction materials are analyzed.
Furthermore, a cooling water pipe is wound outside the condenser 7, and condensed water is introduced into the cooling water pipe.
Condensed water is introduced into a cooling water pipe of the condenser 7, so that the temperature of gas in the condenser can be reduced to below 30 ℃, and the condenser is used for condensing unreacted trichlorosilane and vaporized vinyl trichlorosilane.
An acetylene gas inlet pipe 13 is arranged at the acetylene gas inlet 4; and a gas glass rotameter 14 is arranged on the acetylene gas inlet pipe 13 and used for controlling the gas inlet flow of acetylene.
The acetylene gas inlet pipe 13 is provided with the gas glass rotameter 14, the gas glass rotameter 14 can be started during an experiment to accurately adjust the acetylene flow, and the influence of the ratio of acetylene to trichlorosilane experiment materials on the reaction is tested to obtain a proper production ratio.
Further, a dropping funnel is arranged at the trichlorosilane inlet 5; the dropping funnel is a constant pressure dropping funnel 15.
The constant-pressure dropping funnel is used, so that the trichlorosilane can be uniformly added into the vaporizer, and the reaction is more consistent with the conventional industrial production conditions.
The synthesis device of the embodiment enables trichlorosilane to be vaporized and mixed with acetylene to be fed through the vaporizer, controls the flow of acetylene through the gas glass rotor flow meter 14, controls the amount of trichlorosilane through the constant-pressure dropping funnel 15, and leads water to cool through the glass coil pipe, strictly controls the reaction temperature, so that the reaction synthesis has the advantages of easy operation control, good reaction effect, high product yield and reliable use of the device.
It is to be understood that the above embodiments are merely exemplary embodiments that have been employed to illustrate the principles of the present invention, and that the present invention is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (10)
1. The vinyl trichlorosilane synthesis device is characterized by comprising a vaporizer and a reactor; the vaporizer is communicated with the reactor through a gas guide pipe;
the vaporizer includes a first heating unit and a vaporizer main body; the first heating unit is used for heating the interior of the vaporizer main body; the vaporizer main body is provided with an acetylene gas inlet and a trichlorosilane inlet and is used for conveying mixed gas of trichlorosilane and acetylene which is added into the vaporizer main body and heated and vaporized by the first heating unit into the reactor through a gas guide pipe;
the reactor comprises a temperature control unit, a condenser and a reactor main body; the gas guide pipe extends into the lower part of the reactor main body; the temperature control unit is arranged at the lower part of the reactor main body and is used for controlling the temperature of the lower part of the reactor main body so as to keep the temperature within a preset temperature range; the condenser is arranged at the upper part of the reactor main body and is used for condensing the gas at the upper part of the reactor main body.
2. The synthesis device according to claim 1,
the vaporizer main body is a first multi-mouth flask; the first heating unit is a heating sleeve and is arranged at the bottom of the first multi-mouth flask; the vaporizer also comprises a first temperature measuring instrument which is used for measuring the internal temperature of the first multi-mouth flask;
the reactor main body comprises a second multi-mouth flask and a glass cylinder, and the glass cylinder is arranged at the lower part of the second multi-mouth flask and communicated with the second multi-mouth flask; the temperature control unit comprises a heater, a second temperature measuring instrument and a cooler, wherein the heater is used for heating the reactant in the glass cylinder, the second temperature measuring instrument is used for measuring the temperature of the reactant in the glass cylinder, and the cooler is used for cooling the reactant in the glass cylinder when the temperature of the reactant is higher than a preset temperature value; the condenser is arranged at the upper part of the second multi-mouth flask and is communicated with the second multi-mouth flask.
3. The synthesis device according to claim 2, wherein the gas-guide tube extends into the bottom of the glass cylinder; the lower end of the gas guide pipe is provided with a gas distributor.
4. The synthesis device of claim 2, wherein the heater is an electrical heating tape wrapped around the outside of the glass cylinder.
5. The synthesis device of claim 2, wherein the cooler is a glass coil embedded inside the glass cylinder, and cooling water is introduced into the glass coil to cool the glass cylinder.
6. The synthesis device according to claim 2, wherein the measuring end of the first thermometer extends into the first multi-neck flask from the upper part of the first multi-neck flask; and the measuring end of the second thermometer extends into the bottom of the second multi-mouth flask from the upper part of the second multi-mouth flask and continues to extend into the glass cylinder.
7. The synthesis device according to claim 2, wherein the bottom of the glass cylinder is provided with a discharge valve and a discharge port.
8. The synthesizer according to claim 2, wherein a cooling water pipe is wound around the outside of the condenser, and condensed water is introduced into the cooling water pipe.
9. The synthesis apparatus according to any one of claims 1 to 8, wherein an acetylene gas inlet pipe is provided at the acetylene gas inlet; and a gas glass rotameter is arranged on the acetylene gas inlet pipe and used for controlling the gas inlet flow of acetylene.
10. The synthesis device according to any one of claims 1 to 8, wherein a dropping funnel is arranged at the trichlorosilane inlet; the dropping funnel is a constant pressure dropping funnel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921945730.3U CN211411975U (en) | 2019-11-12 | 2019-11-12 | Vinyl trichlorosilane synthesizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921945730.3U CN211411975U (en) | 2019-11-12 | 2019-11-12 | Vinyl trichlorosilane synthesizer |
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| Publication Number | Publication Date |
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| CN211411975U true CN211411975U (en) | 2020-09-04 |
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| CN201921945730.3U Active CN211411975U (en) | 2019-11-12 | 2019-11-12 | Vinyl trichlorosilane synthesizer |
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Assignee: Xinte silicon based new materials Co.,Ltd. Assignor: XINTE ENERGY Co.,Ltd. Contract record no.: X2023990000586 Denomination of utility model: Vinyl Tri Chlorosilane Synthesis Unit Granted publication date: 20200904 License type: Common License Record date: 20230605 |