阅读说明：本技术 一种聚甲基三乙氧基硅烷管道化连续生产工艺 (Continuous production process of polymethyltriethoxysilane in pipeline mode ) 是由 郑启波 于 2020-04-13 设计创作，主要内容包括：本发明公开了一种聚甲基三乙氧基硅烷管道化连续生产工艺,通过特制盘管反应器,分别将乙醇和一甲基三氯硅烷通入盘管反应器内,快速反应生成聚甲基三乙氧基硅烷,同时产生氯化氢气体,再通过气液分离器分离,制得聚甲基三乙氧基硅烷。由于瞬时使用的主要原料的绝对量大大减少,安全风险大大降低,生产效率大幅度提高。整个生产工艺无需预热,耗时短,安全简单高效。(The invention discloses a pipeline continuous production process of polymethyltriethoxysilane, which comprises the steps of respectively introducing ethanol and methyltrichlorosilane into a special coil reactor, rapidly reacting to generate polymethyltriethoxysilane, simultaneously generating hydrogen chloride gas, and separating by a gas-liquid separator to obtain the polymethyltriethoxysilane. Because the absolute quantity of the main raw materials used instantly is greatly reduced, the safety risk is greatly reduced, and the production efficiency is greatly improved. The whole production process does not need preheating, is short in time consumption, safe, simple and efficient.)

1. A polymethyltriethoxysilane pipelining continuous production process is characterized by comprising the following steps:

(1) customizing a coil reactor: making the pipeline into a coil pipe, filling filler in the coil pipe, and placing the coil pipe in an electric heating barrel;

(2) preheating a coil reactor: the electric heating barrel is filled with water and preheated to 60-90 ℃;

(3) mixing reaction raw materials: the coil pipe is connected with an ethanol metering pump and a methyl trichlorosilane metering pump, the ethanol metering pump is started firstly, ethanol is pumped into the coil pipe reactor, then the methyl trichlorosilane metering pump is started, methyl trichlorosilane is pumped into the coil pipe reactor, the ethanol and the methyl trichlorosilane are fully contacted in the pipeline, the polymethyl triethoxy silane is generated through rapid reaction, and hydrogen chloride gas is generated at the same time;

(4) gas-liquid separation: introducing the polymethyltriethoxysilane and hydrogen chloride gas into a gas-liquid separator, allowing the hydrogen chloride gas to escape upwards and flow into a tail gas absorption tower, and allowing the polymethyltriethoxysilane to flow into a crude product storage tank;

(5) and (3) fine product preparation: and refining the crude product of the polymethyl triethoxy silane to obtain a polymethyl triethoxy silane product.

2. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: the pipeline is DN20, and the length of the pipeline is 30-80 meters.

3. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: the filler is a ceramic ring or a glass spring.

4. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: the flow rate of the methyl trichlorosilane and the ethanol which are pumped into the coil reactor is 150-300 kmol/h.

5. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: the molar ratio of the monomethyl trichlorosilane to the ethanol which are pumped into the coil reactor is 1: 25-1: 35.

6. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: and a guide plate is arranged in the gas-liquid separator, the guide plate is of a spiral rising structure, and hydrogen chloride gas is upwards escaped from the gas-liquid separator along the guide plate.

7. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: the top of the gas-liquid separator is provided with a baffle plate, the baffle plate is provided with air holes, and hydrogen chloride gas flows upwards through the air holes on the baffle plate.

8. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: bottom in the vapour and liquid separator is equipped with agitating unit, agitating unit is including fixing the motor of vapour and liquid separator side with be located solid fixed ring in the vapour and liquid separator, gu fixed ring's upper and lower side all is equipped with the stirring thick liquid, the liquid mixture that the hot coil pipe reactor flows passes through the stirring of stirring thick liquid fully reacts.

9. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: the temperature in the gas-liquid separator is kept between 60 and 90 ℃.

10. The continuous production process of polymethyltriethoxysilane in pipeline form as claimed in claim 1, wherein: and a pump valve is arranged between the coil reactor and the gas-liquid separator.

Technical Field

The invention belongs to the technical field of polymethyl triethoxy silane production, and particularly relates to a pipelining continuous production process of polymethyl triethoxy silane.

Background

Polymethyl triethoxy silane is used in rubber and medicine industry as organic silicon polymer material. The product is an important raw material for producing silicone resin, benzyl silicone oil and a waterproof agent. And meanwhile, the silicon alkoxide is easy to hydrolyze and can generate alkali metal silicon alkoxide with alkali metal hydroxide. And can also be used as a cross-linking agent for room temperature vulcanized silicone rubber.

The conventional method for synthesizing the polymethyltriethoxysilane is to inject metered monomethyltrichlorosilane into a reaction kettle, heat the mixture to 60-90 ℃, dropwise add anhydrous ethanol into the kettle from an anhydrous ethanol elevated tank, and introduce nitrogen for bubbling to perform reflux reaction. In the heating reflux reaction process, the monomethyl trichlorosilane reacts with absolute ethyl alcohol to generate polymethyl triethoxy silane and hydrogen chloride, the ascending gas flow enters a condenser, the condensate flows back to the reaction kettle, and the uncondensed gas hydrogen chloride is absorbed by tail gas. After the reaction is finished, the residual reaction liquid in the kettle is the polymethyl triethoxy silane product. The production method has high safety risk, a large amount of monomethyl trichlorosilane required by each batch of reaction is completely injected into the reaction kettle at one time, and the explosion risk caused by static electricity exists; the risk of material leakage is difficult to prevent and control when the equipment is damaged; the reaction period is long, more than 30 hours are consumed for one batch of materials, and the production efficiency is low.

Disclosure of Invention

The invention aims to provide a polymethyltriethoxysilane pipelining continuous production process, which greatly reduces the absolute amount of main raw materials used instantly, greatly reduces the safety risk, greatly improves the production efficiency, greatly reduces the number of workers and labor intensity, and has uniform and stable product quality.

In order to solve the technical problems, the invention adopts the following technical scheme:

a polymethyltriethoxysilane pipelining continuous production process is characterized by comprising the following steps:

(1) customizing a coil reactor: making the pipeline into a coil pipe, filling filler in the coil pipe, and placing the coil pipe in an electric heating barrel;

(2) preheating a coil reactor: the electric heating barrel is filled with water and preheated to 60-90 ℃;

(3) mixing reaction raw materials: the coil pipe is connected with an ethanol metering pump and a methyl trichlorosilane metering pump, the ethanol metering pump is started firstly, ethanol is pumped into the coil pipe reactor, then the methyl trichlorosilane metering pump is started, methyl trichlorosilane is pumped into the coil pipe reactor, the ethanol and the methyl trichlorosilane are fully contacted in a pipeline, the polymethyl triethoxy silane is generated through rapid reaction, and hydrogen chloride gas is generated at the same time;

(4) gas-liquid separation: introducing the polymethyltriethoxysilane and hydrogen chloride gas into a gas-liquid separator, allowing the hydrogen chloride gas to escape upwards and flow into a tail gas absorption tower, and allowing the polymethyltriethoxysilane to flow into a crude product storage tank;

(5) and (3) fine product preparation: and refining the crude product of the polymethyl triethoxy silane to obtain a polymethyl triethoxy silane product.

The ethanol and the monomethyl trichlorosilane instantaneously react in the coil reactor to generate the polymethyl triethoxy silane, and because the absolute amount of the instantaneously used main raw materials is greatly reduced, the safety risk is greatly reduced, and the production efficiency is greatly improved. The polymethyl triethoxy silane and hydrogen chloride gas generated by the reaction are separated by a gas-liquid separator, the hydrogen chloride gas escapes upwards, and the polymethyl triethoxy silane flows out from the bottom of the gas-liquid separator. The whole production process does not need preheating, is short in time consumption, safe, simple and efficient.

Preferably, the pipeline is DN20, and the length of the pipeline is 30-80 meters.

Preferably, the filler is a ceramic ring or a glass spring. The filler increases resistance, and plays a role in stirring the ethanol and the monomethyl trichlorosilane, so that the ethanol and the monomethyl trichlorosilane are fully mixed. Because hydrogen chloride gas is generated in the reaction process, the ceramic ring and the glass spring cannot be corroded by the hydrogen chloride gas.

Preferably, the flow rates of the monomethyl trichlorosilane and the ethanol which are pumped into the coil reactor are both 150-300 kmol/h.

Preferably, the mol ratio of the monomethyltrichlorosilane to the ethanol which is pumped into the coil reactor is 1: 25-1: 35.

Preferably, a guide plate is arranged in the gas-liquid separator, the guide plate is of a spiral rising structure, and hydrogen chloride gas upwards escapes from the gas-liquid separator along the guide plate. The mixed solution in the coil reactor flows into the gas-liquid separator, the hydrogen chloride gas flows upwards along the guide plate, and the liquid flows downwards to the bottom of the gas-liquid separator.

Preferably, the top of the gas-liquid separator is provided with a baffle plate, the baffle plate is provided with air holes, and hydrogen chloride gas flows upwards through the air holes on the baffle plate. The baffle is used for blocking liquid entrained in the gas.

Preferably, the bottom in the gas-liquid separator is provided with a stirring device, the stirring device comprises a motor fixed on the side of the gas-liquid separator and a fixing ring positioned in the gas-liquid separator, the upper side and the lower side of the fixing ring are both provided with stirring paddles, and the liquid mixture flowing out of the hot coil reactor is fully reacted through the stirring of the stirring paddles. The residual ethanol and the monomethyl trichlorosilane may be remained in the inflowing liquid, and the unreacted ethanol and the monomethyl trichlorosilane are fully mixed by the stirring device, so that the yield of the raw materials is improved. And the stirring process facilitates the escape of hydrogen chloride gas.

Preferably, the temperature in the gas-liquid separator is maintained at 60 to 90 ℃.

Preferably, a pump valve is arranged between the coil reactor and the gas-liquid separator. When raw materials are introduced into the coil reactor, the valve is opened, and when the raw materials in the coil reactor are introduced into the gas-liquid separator, the pump is opened.

Due to the adoption of the technical scheme, the invention has the following beneficial effects:

the ethanol and the monomethyl trichlorosilane instantaneously react in the coil reactor to generate the polymethyl triethoxy silane, and because the absolute amount of the instantaneously used main raw materials is greatly reduced, the safety risk is greatly reduced, and the production efficiency is greatly improved. The polymethyl triethoxy silane and hydrogen chloride gas generated by the reaction are separated by a gas-liquid separator, the hydrogen chloride gas escapes upwards, and the polymethyl triethoxy silane flows out from the bottom of the gas-liquid separator. The filler increases resistance, and plays a role in stirring the ethanol and the monomethyl trichlorosilane, so that the ethanol and the monomethyl trichlorosilane are fully mixed. Because hydrogen chloride gas is generated in the reaction process, the ceramic ring and the glass spring cannot be corroded by the hydrogen chloride gas. The hydrogen chloride in the gas-liquid separator overflows upwards through the guide plate, and the solution is stirred by the stirring paddle to fully react the unreacted raw materials. The whole production process has the advantages of low energy consumption, short consumed time, simple operation, great reduction of the number of workers and the labor intensity, and uniform and stable product quality.

Drawings

The invention is further illustrated below with reference to the accompanying drawings.

FIG. 1 is a process flow diagram of a continuous pipeline production process of polymethyltriethoxysilane in the present invention.

Detailed Description

The pipeline continuous production device of the polymethyltriethoxysilane shown in figure 1 comprises a coil reactor 1, a gas-liquid separator 2, a crude product storage tank (not shown in the figure) and a tail gas absorption tower 3. The coil reactor 1 comprises a coil 4 and an electric heating barrel 5, the top of the coil 4 is connected with a control valve 6, two sides of the control valve 6 are respectively connected with an ethanol metering pump 7 and a methyl trichlorosilane metering pump 8, and the control valve 6 is used for controlling the introduction of ethanol or methyl trichlorosilane. The bottom of the coil 4 is connected with the pump valve 9 and the gas-liquid separator 2 through pipelines. The top of the electric heating barrel 5 is provided with a water inlet 10 and a thermometer 11. The top of the gas-liquid separator 2 is connected with the tail gas absorption tower 3, and the bottom of the gas-liquid separator 2 is connected with the discharge valve and the crude product storage tank. When the raw materials are introduced into the reactor 1 of the coil 4, the valve is opened, and when the raw materials in the reactor 1 of the coil 4 are introduced into the gas-liquid separator 2, the pump is opened.

A guide plate 12 is arranged in the gas-liquid separator 2, the guide plate 12 is of a spiral rising structure, and hydrogen chloride gas escapes from the gas-liquid separator 2 upwards along the guide plate 12. The mixed solution in the coil 4 reactor 1 flows into the gas-liquid separator 2, the hydrogen chloride gas flows upwards along the guide plate 12, and the liquid flows downwards to the bottom of the gas-liquid separator 2. The top of the gas-liquid separator 2 is provided with a baffle 13, the baffle 13 is provided with air holes, and hydrogen chloride gas flows upwards through the air holes on the baffle 13. The baffle 13 is used to trap liquid entrained in the gas.

The bottom in the vapour and liquid separator 2 is equipped with agitating unit, and agitating unit is including fixing motor 14 and the solid fixed ring 15 that is located the vapour and liquid separator 2 of vapour and liquid separator 2 side, and solid fixed ring 15's upper and lower side all is equipped with stirring rake 16. The motor 14 is started to drive the stirring paddle 16 to rotate, and the liquid mixture flowing out of the reactor 1 of the hot coil 4 is fully reacted by stirring of the stirring paddle 16. The residual ethanol and the monomethyl trichlorosilane may be remained in the inflowing liquid, and the unreacted ethanol and the monomethyl trichlorosilane are fully mixed by the stirring device, so that the yield of the raw materials is improved. And the stirring process facilitates the escape of hydrogen chloride gas.

A polymethyl triethoxy silane pipelining continuous production process comprises the following steps:

(1) custom coil 4 reactor 1: the pipeline is DN20, the length of the pipeline is 30-80 meters, the pipeline is made into a coil 4, the coil 4 is filled with filling materials, and the coil 4 is placed in an electric heating barrel 5;

(2) preheating coil 4 reactor 1: the electric heating barrel 5 is filled with water and preheated to 60-90 ℃;

(3) mixing reaction raw materials: the coil 4 is connected with an ethanol metering pump 7 and a methyltrichlorosilane metering pump 8, the ethanol metering pump 7 is started firstly, ethanol is injected into the reactor 1 of the coil 4, the methyltrichlorosilane metering pump 8 is started, the methyltrichlorosilane is injected into the reactor 1 of the coil 4, the ethanol and the methyltrichlorosilane are fully contacted in a pipeline, the polymethyltriethoxysilane is generated through rapid reaction, hydrogen chloride gas is generated simultaneously, the flow rate of the ethanol and the monomethyltrichlorosilane injected into the reactor 1 of the coil 4 is 150 kmol/h-300 kmol/h, and the molar ratio of the ethanol to the monomethyltrichlorosilane injected into the reactor 1 of the coil 4 is 1: 25-1: 35;

(4) gas-liquid separation: introducing polymethyl triethoxy silane and hydrogen chloride gas into a gas-liquid separator 2, keeping the temperature in the gas-liquid separator 2 at 60-90 ℃, enabling the hydrogen chloride gas to flow upwards to a baffle 13 through a guide plate 12, enabling the hydrogen chloride gas to escape through air holes of the baffle 13 and flow into a tail gas absorption tower 3, and blocking liquid carried by the hydrogen chloride gas by the baffle 13 and the guide plate 12; the polymethyl triethoxy silane and unreacted raw materials are placed at the bottom of the gas-liquid separator 2, the liquid is stirred by the stirring paddle 16, the hydrogen chloride generated by the reaction of the unreacted raw materials flows upwards, the stirring speed is 100r/min-200r/min, and after the stirring is finished, the polymethyl triethoxy silane flows into a crude product storage tank;

(5) and (3) fine product preparation: and refining the crude product of the polymethyl triethoxy silane to obtain a polymethyl triethoxy silane product.

Wherein the filler is a ceramic ring or a glass spring. The filler increases resistance, and plays a role in stirring the ethanol and the monomethyl trichlorosilane, so that the ethanol and the monomethyl trichlorosilane are fully mixed. Because hydrogen chloride gas is generated in the reaction process, the ceramic ring and the glass spring cannot be corroded by the hydrogen chloride gas.