Preparation method of ethyl lactate silane and reaction device
The membrane reaction unit in the ethyl lactate silane production process absorbs hydrogen chloride to form ammonium chloride salt particles, addressing wastewater and quality issues, resulting in high-purity ethyl lactate silane with reduced environmental impact and increased efficiency.
Patent Information
- Application Number
- CN202411306892.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-19
- Publication Date
- 2025-01-03
AI Technical Summary
The production of ethyl lactate silane using acid-binding agents like triethylamine generates amine-containing wastewater and results in poor product quality due to residual amines, leading to environmental pollution and increased energy consumption.
A method and device utilizing a membrane reaction unit where ammonia gas enters through membrane pores to absorb hydrogen chloride, forming ammonium chloride salt particles, which are then separated from the crude product, eliminating the need for triethylamine and reducing wastewater generation.
This approach produces ethyl lactate silane with high purity and quality, reduces wastewater treatment steps, is environmentally friendly, and enhances production efficiency by improving ammonia mass transfer and reaction rates.
Smart Images
Figure CN119236861A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical synthesis, and in particular to a preparation method and a reaction device of ethyl lactate silane. Background Art
[0002] Ethyl lactate silane is used as a crosslinking agent to prepare room temperature curing silicone rubber. Ethyl lactate silanes such as methyl triethyl lactate silane, vinyl triethyl lactate silane, tetraethyl lactate silane, etc., have a pleasant fruity aroma when crosslinked, and ethyl lactate is friendly to people. Therefore, ethyl lactate silane is an environmentally friendly silane crosslinking agent and a silane crosslinking agent for the future market.
[0003] At present, ethyl lactate type silane cross-linking agent adopts ethyl lactate and chlorosilane to react under negative pressure at room temperature to make, and the above-mentioned reaction can produce hydrogen chloride, and the activity of ethyl lactate is higher, hydrogen chloride gas can not be discharged in time and is prone to side reaction, affects the quality of product, in order to promote reaction and timely remove hydrogen chloride, need to improve reaction temperature and excessive use of ethyl lactate, but this can cause product polymerization side reaction to increase, and feedstock conversion is low, energy consumption is high. Therefore in order to solve the above problem, disclose in the prior art to use and add acid binding agent to absorb the hydrogen chloride produced, as triethylamine has been adopted as acid binding agent to absorb hydrogen chloride in publication number US10590151B2 and publication number US8569439B2.But using triethylamine as acid binding agent can produce a large amount of amine-containing toxic waste water, seriously pollutes environment, and also contains trace triethylamine in the product obtained, makes product produce peculiar smell, affects product quality. Summary of the invention
[0004] In order to overcome the problem that the use of acid-binding agents in the production process of ethyl lactate silane in the prior art will generate a large amount of amine-containing wastewater and poor product quality, the present invention provides a preparation method and reaction device for ethyl lactate silane, which uses a membrane reaction unit to make the reaction materials flow and react at a high speed in the narrow space inside the membrane, and the ammonia outside the membrane enters the membrane inside through the membrane pores to absorb the hydrogen chloride generated by the reaction to generate ammonium chloride salt particles, and then the ammonium chloride salt particles and solvent oil in the crude product are separated to obtain the ethyl lactate silane product. The product obtained by this method will not have residual amines, and the product quality is high; the method will not generate a large amount of amine-containing wastewater, reduce the steps of amine-containing wastewater treatment, is environmentally friendly and energy-saving, and significantly improves production efficiency; in addition, the membrane reaction component can also improve the ammonia mass transfer efficiency, improve the material reaction rate and material conversion rate.
[0005] The specific technical scheme of the present invention is: A method for preparing ethyl lactate silane comprises the following steps: introducing ammonia into a shell, injecting solvent oil, ethyl lactate and chlorosilane into a membrane reaction component in the shell for reaction to obtain a crude product, filtering and distilling the crude product to obtain ethyl lactate silane; the membrane reaction unit comprises a hollow frame and a membrane arranged on the hollow frame, and the pore size of the membrane is 0.1-1 μm.
[0006] Preferably, the mass ratio of solvent oil to chlorosilane is 3-8:1, and the molar ratio of ethyl lactate to chlorine in chlorosilane is 1-1.01:1.
[0007] Preferably, the pressure of the ammonia gas is 100-200 KPa, the reaction temperature is 30-60° C., and the pH of the crude product is 7-13.
[0008] Preferably, the chlorosilane is one or more of methyltrichlorosilane, vinyltrichlorosilane, phenyltrichlorosilane or silicon tetrachloride.
[0009] The invention provides a method for preparing ethyl lactate silane. The method uses a membrane reaction unit to make the reaction materials flow at a high speed in a narrow space inside the membrane for reaction. Ammonia gas outside the membrane enters the membrane inside through the membrane pores to absorb hydrogen chloride generated by the reaction to generate ammonium chloride salt particles. The ammonium chloride salt particles and the oil solvent in the crude product are then separated to obtain the ethyl lactate silane product. The pore size of the membrane is used to prevent the reaction materials from passing through the membrane while ammonia gas can enter the pore structure of the membrane. When the reaction materials react to generate hydrogen chloride, the ammonia gas entering from the membrane pores will react with the hydrogen chloride to generate ammonium chloride salt particles. The ammonium chloride salt is generated by the reaction and is in the form of crystal particles in the reaction material. Compared with the technical solution of directly adding triethylamine, a large amount of amine-containing wastewater will not be generated, and there is no need to treat the amine-containing wastewater. It is environmentally friendly and energy-saving, and the production efficiency is increased. In addition, excessive triethylamine will remain in the product in trace amounts, causing the product quality to deteriorate. The product prepared by the present application has no residue, the ethyl lactate content is reduced, and the purity is significantly improved. In addition, the space of the membrane reaction component in the method is narrow, the reaction rate of the reaction material is fast in the narrow reaction space, the material conversion rate is high, and the mass transfer efficiency is high.
[0010] A reaction device comprises a shell and a membrane reaction component arranged in the shell, wherein the membrane reaction component comprises a plurality of membrane reaction units connected to each other, and the shell and the membrane reaction component are the shell and the membrane reaction component in the above-mentioned method for preparing ethyl lactate silane.
[0011] Preferably, the membrane reaction unit comprises a hollow frame and a membrane arranged on the hollow frame, windows are arranged on both side surfaces of the hollow frame, the membrane is detachably connected to the window, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, and a buckle detachably connected to the card slot is arranged on the support frame.
[0012] Preferably, the spacing between membranes in the membrane reaction unit is 1 to 5 mm.
[0013] Preferably, the spacing between the membrane reaction units is 50 to 200 mm.
[0014] Preferably, the width of the membrane reaction unit is 5 to 200 mm.
[0015] Preferably, the aspect ratio of the membrane reaction unit is greater than 2.
[0016] Preferably, the shell is provided with an air inlet, a liquid inlet and a liquid outlet, the liquid outlet is provided with a pH detection device, the liquid outlet is connected to a filtering and distilling device, the liquid inlet is connected to a chlorosilane feeder, a lactate feeder and a heat exchange device, the heat exchange device is connected to a solvent oil feeder, and a temperature tester and a pressure tester are provided inside the shell.
[0017] Preferably, the filtering and distilling device comprises a tank body and a filter screen arranged on the top of the tank body.
[0018] Preferably, a scraper is provided on the filter screen.
[0019] The present invention also provides a reaction device, which consists of a shell and a membrane reaction component arranged in the shell, the membrane reaction component consists of a plurality of interconnected membrane reaction units, and the membrane reaction unit consists of a hollow frame and a membrane arranged on the frame. When the device is in use, ammonia gas is introduced into the shell, and mixed raw materials are introduced into the hollow frame. The membrane can pass through the gas to block the liquid. Therefore, when the reaction liquid in the hollow frame reacts, the ammonia gas in the shell can react with the hydrogen chloride generated in the reaction material through the membrane to generate ammonium chloride, so that the hydrogen chloride generated in the hollow frame is quickly neutralized, and the utilization rate of the ammonia gas can reach 100%; the reaction does not use triethylamine as an acid binding agent, does not need to be neutralized and recovered triethylamine, and does not generate a large amount of triethylamine-containing wastewater. In addition, the reaction materials flow at high speed in the narrow gap of the hollow frame, the liquid holding capacity is small, the mixing effect, the mass transfer effect and the reaction speed are significantly improved, and when a certain molar ratio of chlorosilane and lactate is used, the chlorosilane can be completely reacted, and the lactate content in the obtained crude product is low. The product can be purified quickly at a relatively low temperature, the purification time is short, the energy consumption is reduced, and the obtained product has high purity and good chromaticity.
[0020] Compared with the prior art, this application has the following technical effects: The invention provides a preparation method and a reaction device of ethyl lactate silane. The device consists of a shell and a membrane reaction component arranged in the shell. The membrane reaction component consists of a plurality of connected membrane reaction units. The method adopts the method of allowing reaction materials to flow and react in a narrow space inside a membrane through the membrane reaction unit, and ammonia outside the membrane enters the inside of the membrane through membrane pores to absorb hydrogen chloride generated by the reaction to generate ammonium chloride salt particles, and then the ammonium chloride salt particles and solvent oil in the crude product are separated to obtain the ethyl lactate silane product. The method does not use triethylamine as an acid binding agent, and the obtained product does not have residual amines and has high product quality. The method does not generate a large amount of amine-containing wastewater, reduces the steps of treating the amine-containing wastewater, is environmentally friendly and energy-saving, and significantly improves production efficiency. In addition, the membrane reaction component can also improve the ammonia mass transfer efficiency, improve the material reaction rate and the material conversion rate, and obtain a product with high purity and good chromaticity. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 It is a cross-sectional view of the reaction device of the present invention.
[0022] Figure 2 It is a cross-sectional view of the membrane reaction unit of the present invention.
[0023] In the figure, there are a shell 1, an air inlet 101, a liquid inlet 103, a liquid outlet 104, a pH detection device 105, a heat exchange device 107, an oil solvent feeder 108, a chlorosilane feeder 109, a lactate feeder 110, a temperature tester 111, a pressure tester 112, a membrane reaction assembly 2, a membrane reaction unit 201, a hollow frame 211, a membrane 212 and a window 213. DETAILED DESCRIPTION
[0024] The present invention will be further described below in conjunction with the embodiments.
[0025] Embodiment 1: A reaction device, such as Figure 1 As shown, it includes a shell 1 and a membrane reaction assembly 2 arranged in the shell, the membrane reaction assembly includes 40 connected membrane reaction units, the membrane reaction unit length is 1000mm, the width is 200mm; the spacing between the membrane reaction units is 50mm, the shell is provided with an air inlet 101, a liquid inlet 103 and a liquid outlet 104, the liquid outlet is provided with a pH detection device 105, the liquid outlet is connected to a filtering distillation device, the filtering distillation device includes a tank body and a filter screen arranged in the tank body, the filtering accuracy of the filter screen is 1μm, and a scraper is provided at the bottom of the filter screen. The scraper scrapes off the ammonium chloride on the filter screen under the drive of a motor to prevent the ammonium chloride from agglomerating on the filter screen; the liquid inlet is connected to a chlorosilane feeder 109, a lactate feeder 110 and a heat exchange device 107, the heat exchange device is connected to an oil solvent feeder 108, and a temperature tester 111 and a pressure tester 112 are provided inside the shell; like Figure 2As shown, the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, the pore size of the membrane is 0.1 μm, windows are arranged on both side surfaces of the frame, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, a buckle which is detachably connected to the card slot is arranged on the support frame, and the membrane spacing on adjacent windows is 2 mm.
[0026] A method for preparing ethyl lactate silane, using the above reaction device, comprises the following steps: The oil solvent is cooled through a heat exchange device at a feed rate of 1500L / h and then injected into the liquid inlet. Vinyltrichlorosilane is injected into the liquid inlet from a chlorosilane feeder at a feed rate of 130kg / h and ethyl lactate is injected into the liquid inlet from a lactate feeder at a feed rate of 287kg / h, respectively. The air inlet is opened to allow ammonia gas to enter the shell from the air inlet, and the ammonia pressure is controlled to be 100KPa. The temperature of the solvent oil is adjusted by adjusting the refrigerant amount of the solvent oil heat exchanger through a temperature tester to adjust the temperature of the solvent oil so as to control the reaction temperature to be 40-45°C for reaction. The pH of the crude product is detected by a pH detection device on the liquid outlet. After the crude product flows out, it enters a filtration distillation device to remove ammonium chloride salt particles in the crude product by filtration, and the product ethyl lactate silane is obtained by distillation under the conditions of a distillation temperature of 100°C and a distillation pressure of 750mmHg.
[0027] Embodiment 2: A reaction device, such as Figure 1 As shown, it includes a shell 1 and a membrane reaction assembly 2 arranged in the shell, the membrane reaction assembly includes 40 connected membrane reaction units, the membrane reaction unit length is 1000mm, the width is 200mm; the spacing between the membrane reaction units is 50mm, the shell is provided with an air inlet 101, a liquid inlet 103 and a liquid outlet 104, the liquid outlet is provided with a pH detection device 105, the liquid outlet is connected to a filtering distillation device, the filtering distillation device includes a tank body and a filter screen arranged in the tank body, the filtering accuracy of the filter screen is 1μm, and a scraper is provided at the bottom of the filter screen. The scraper scrapes off the ammonium chloride on the filter screen under the drive of a motor to prevent the ammonium chloride from agglomerating on the filter screen; the liquid inlet is connected to a chlorosilane feeder 109, a lactate feeder 110 and a heat exchange device 107, the heat exchange device is connected to an oil solvent feeder 108, and a temperature tester 111 and a pressure tester 112 are provided inside the shell; like Figure 2 As shown, the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, the pore size of the membrane is 0.1μm, windows are arranged on both side surfaces of the frame, card slots are arranged on the windows, a support frame is arranged on the outer edge of the membrane, a buckle which is detachably connected to the card slot is arranged on the support frame, and the membrane spacing on adjacent windows is 4mm.
[0028] A method for preparing ethyl lactate silane, using the above reaction device, comprises the following steps: The oil solvent is cooled through a heat exchange device at a feed rate of 1500L / h and then injected into the liquid inlet. Vinyltrichlorosilane is injected into the liquid inlet from a chlorosilane feeder at a feed rate of 130kg / h and ethyl lactate is injected into the liquid inlet from a lactate feeder at a feed rate of 287kg / h, respectively. The air inlet is opened to allow ammonia gas to enter the shell from the air inlet, and the ammonia pressure is controlled to be 100KPa. The temperature of the solvent oil is adjusted by adjusting the refrigerant amount of the solvent oil heat exchanger through a temperature tester to adjust the temperature of the solvent oil so as to control the reaction temperature to be 40-45°C for reaction. The pH of the crude product is detected by a pH detection device on the liquid outlet. After the crude product flows out, it enters a filtration distillation device to remove ammonium chloride salt particles in the crude product by filtration, and the product ethyl lactate silane is obtained by distillation under the conditions of a distillation temperature of 100°C and a distillation pressure of 750mmHg.
[0029] Embodiment 3: A reaction device, such as Figure 1 As shown, it includes a shell 1 and a membrane reaction assembly 2 arranged in the shell, the membrane reaction assembly includes 40 connected membrane reaction units, the membrane reaction unit length is 1000mm, the width is 200mm; the spacing between the membrane reaction units is 100mm, the shell is provided with an air inlet 101, a liquid inlet 103 and a liquid outlet 104, the liquid outlet is provided with a pH detection device 105, the liquid outlet is connected to a filtering distillation device, the filtering distillation device includes a tank body and a filter screen arranged in the tank body, the filtering accuracy of the filter screen is 1μm, and a scraper is provided at the bottom of the filter screen. The scraper scrapes off the ammonium chloride on the filter screen under the drive of a motor to prevent the ammonium chloride from agglomerating on the filter screen; the liquid inlet is connected to a chlorosilane feeder 109, a lactate feeder 110 and a heat exchange device 107, the heat exchange device is connected to an oil solvent feeder 108, and a temperature tester 111 and a pressure tester 112 are provided inside the shell; like Figure 2 As shown, the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, the pore size of the membrane is 0.22μm, windows are arranged on both side surfaces of the frame, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, a buckle which is detachably connected to the card slot is arranged on the support frame, and the membrane spacing on adjacent windows is 3mm.
[0030] A method for preparing ethyl lactate silane, using the above reaction device, comprises the following steps: The oil solvent is cooled through a heat exchange device at a feed rate of 1500L / h and then injected into the liquid inlet. Vinyltrichlorosilane is injected into the liquid inlet from a chlorosilane feeder at a feed rate of 130kg / h and ethyl lactate is injected into the liquid inlet from a lactate feeder at a feed rate of 287kg / h, respectively. The air inlet is opened to allow ammonia gas to enter the shell from the air inlet, and the ammonia pressure is controlled to be 100KPa. The temperature of the solvent oil is adjusted by adjusting the refrigerant amount of the solvent oil heat exchanger through a temperature tester to adjust the temperature of the solvent oil so as to control the reaction temperature to be 40-45°C for reaction. The pH of the crude product is detected by a pH detection device on the liquid outlet. After the crude product flows out, it enters a filtration distillation device to remove ammonium chloride salt particles in the crude product by filtration, and the product ethyl lactate silane is obtained by distillation under the conditions of a distillation temperature of 100°C and a distillation pressure of 750mmHg.
[0031] Embodiment 4: A reaction device, such as Figure 1 As shown, it includes a shell 1 and a membrane reaction assembly 2 arranged in the shell, the membrane reaction assembly includes 40 connected membrane reaction units, the membrane reaction unit length is 1000mm, the width is 200mm; the spacing between the membrane reaction units is 50mm, the shell is provided with an air inlet 101, a liquid inlet 103 and a liquid outlet 104, the liquid outlet is provided with a pH detection device 105, the liquid outlet is connected to a filtering distillation device, the filtering distillation device includes a tank body and a filter screen arranged in the tank body, the filtering accuracy of the filter screen is 1μm, and a scraper is provided at the bottom of the filter screen. The scraper scrapes off the ammonium chloride on the filter screen under the drive of a motor to prevent the ammonium chloride from agglomerating on the filter screen; the liquid inlet is connected to a chlorosilane feeder 109, a lactate feeder 110 and a heat exchange device 107, the heat exchange device is connected to an oil solvent feeder 108, and a temperature tester 111 and a pressure tester 112 are provided inside the shell; like Figure 2 As shown, the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, the pore size of the membrane is 0.1 μm, windows are arranged on both side surfaces of the frame, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, a buckle which is detachably connected to the card slot is arranged on the support frame, and the membrane spacing on adjacent windows is 2 mm.
[0032] A method for preparing ethyl lactate silane, using the above reaction device, comprises the following steps: The oil solvent is cooled through a heat exchange device at a feed rate of 1500L / h and then injected into the liquid inlet. Methyltrichlorosilane is injected into the liquid inlet from a chlorosilane feeder at a feed rate of 130kg / h and ethyl lactate is injected into the liquid inlet from a lactate feeder at a feed rate of 310kg / h, respectively. The air inlet is opened to allow ammonia gas to enter the shell from the air inlet, and the ammonia pressure is controlled to be 100KPa. The temperature of the solvent oil is adjusted by adjusting the refrigerant amount of the solvent oil heat exchanger through a temperature tester to adjust the temperature of the solvent oil so as to control the reaction temperature to be 40-45°C for reaction. The pH of the crude product is detected by a pH detection device on the liquid outlet. After the crude product flows out, it enters a filtration distillation device to remove ammonium chloride salt particles in the crude product by filtration, and the product ethyl lactate silane is obtained by distillation under the conditions of a distillation temperature of 100°C and a distillation pressure of 750mmHg.
[0033] Embodiment 5: A reaction device, such as Figure 1 As shown, it includes a shell 1 and a membrane reaction assembly 2 arranged in the shell, the membrane reaction assembly includes 40 connected membrane reaction units, the membrane reaction unit length is 1000mm, the width is 200mm; the spacing between the membrane reaction units is 50mm, the shell is provided with an air inlet 101, a liquid inlet 103 and a liquid outlet 104, the liquid outlet is provided with a pH detection device 105, the liquid outlet is connected to a filtering distillation device, the filtering distillation device includes a tank body and a filter screen arranged in the tank body, the filtering accuracy of the filter screen is 1μm, and a scraper is provided at the bottom of the filter screen. The scraper scrapes off the ammonium chloride on the filter screen under the drive of a motor to prevent the ammonium chloride from agglomerating on the filter screen; the liquid inlet is connected to a chlorosilane feeder 109, a lactate feeder 110 and a heat exchange device 107, the heat exchange device is connected to an oil solvent feeder 108, and a temperature tester 111 and a pressure tester 112 are provided inside the shell; like Figure 2 As shown, the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, the pore size of the membrane is 0.1 μm, windows are arranged on both side surfaces of the frame, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, a buckle which is detachably connected to the card slot is arranged on the support frame, and the membrane spacing on adjacent windows is 2 mm.
[0034] A method for preparing ethyl lactate silane, using the above reaction device, comprises the following steps: The oil solvent is cooled through a heat exchange device at a feed rate of 1500L / h and then injected into the liquid inlet. Then, phenyltrichlorosilane is injected into the liquid inlet from a chlorosilane feeder at a feed rate of 170kg / h and ethyl lactate is injected into the liquid inlet from a lactate feeder at a feed rate of 286kg / h. The air inlet is opened to allow ammonia gas to enter the shell from the air inlet, and the ammonia pressure is controlled to be 100KPa. The temperature of the solvent oil is adjusted by adjusting the refrigerant amount of the solvent oil heat exchanger through a temperature tester to adjust the temperature of the solvent oil so as to control the reaction temperature to be 40-45°C for reaction. The pH of the crude product is detected by a pH detection device on the liquid outlet. After the crude product flows out, it enters a filtration distillation device to remove ammonium chloride salt particles in the crude product by filtration, and the product ethyl lactate silane is obtained by distillation under the conditions of a distillation temperature of 100°C and a distillation pressure of 750mmHg.
[0035] Embodiment 6: A reaction device, such as Figure 1 As shown, it includes a shell 1 and a membrane reaction assembly 2 arranged in the shell, the membrane reaction assembly includes 40 connected membrane reaction units, the membrane reaction unit length is 1000mm, the width is 200mm; the spacing between the membrane reaction units is 50mm, the shell is provided with an air inlet 101, a liquid inlet 103 and a liquid outlet 104, the liquid outlet is provided with a pH detection device 105, the liquid outlet is connected to a filtering distillation device, the filtering distillation device includes a tank body and a filter screen arranged in the tank body, the filtering accuracy of the filter screen is 1μm, and a scraper is provided at the bottom of the filter screen. The scraper scrapes off the ammonium chloride on the filter screen under the drive of a motor to prevent the ammonium chloride from agglomerating on the filter screen; the liquid inlet is connected to a chlorosilane feeder 109, a lactate feeder 110 and a heat exchange device 107, the heat exchange device is connected to an oil solvent feeder 108, and a temperature tester 111 and a pressure tester 112 are provided inside the shell; like Figure 2 As shown, the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, the pore size of the membrane is 0.1 μm, windows are arranged on both side surfaces of the frame, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, a buckle which is detachably connected to the card slot is arranged on the support frame, and the membrane spacing on adjacent windows is 2 mm.
[0036] A method for preparing ethyl lactate silane, using the above reaction device, comprises the following steps: The oil solvent is cooled through a heat exchange device at a feed rate of 1500L / h and then injected into the liquid inlet. Then, silicon tetrachloride is injected into the liquid inlet from a chlorosilane feeder at a feed rate of 100kg / h and ethyl lactate is injected into the liquid inlet from a lactate feeder at a feed rate of 210kg / h. The air inlet is opened to allow ammonia gas to enter the shell from the air inlet, and the ammonia pressure is controlled to be 100KPa. The temperature of the solvent oil is adjusted by adjusting the refrigerant amount of the solvent oil heat exchanger through a temperature tester to adjust the temperature of the solvent oil so as to control the reaction temperature to be 40-45°C for reaction. The pH of the crude product is detected by a pH detection device on the liquid outlet. After the crude product flows out, it enters a filtration distillation device to remove ammonium chloride salt particles in the crude product by filtration, and the product ethyl lactate silane is obtained by distillation under the conditions of a distillation temperature of 100°C and a distillation pressure of 750mmHg.
[0037] Comparative Example 1: Compared with Example 1, Comparative Example 1 adopts a direct reaction process of vinyltrichlorosilane and ethyl lactate, comprising the following steps: Vinyl trichlorosilane and ethyl lactate were used in a 1000L standard glass-lined reactor (outer dimensions ) for reaction; first add 250kg of vinyl trichlorosilane into the reactor, then at a temperature of 30-40°C and a negative pressure of -10Kpa, drop 650kg of ethyl lactate into the reactor for reaction, the drop rate is 100kg / h, and the hydrogen chloride generated during the drop reaction is absorbed by water; after the drop addition is completed, the temperature is raised to 80°C and the reaction is continued for 3h; then the reaction product is transferred to a distillation kettle of the same specification, and distilled at a distillation temperature of 100°C and a distillation pressure of 750mmHg to obtain the product ethyl lactate silane, and 605kg of the product is obtained, with a yield of 96.2% (based on chlorosilane); the reaction product detection results: the purity of vinyl triethyl lactate silane is 94.8%, the content of ethyl lactate is 1.78, the color APHA is 50; the chloride ion is 15ppm; the amount of tail gas hydrogen chloride consumed is calculated based on the final generation of 25% hydrochloric acid, and 510kg of water is consumed, equivalent to 0.84 tons / ton of product.
[0038] Comparative Example 2: Compared with Example 1, the process of triethylamine acid binding agent in the prior art was adopted in Comparative Example 1. The following steps are involved: Vinyl trichlorosilane and ethyl lactate were used in a 1000L standard glass-lined reactor (outer dimensions ) for reaction; first add 280g of ethyl lactate and 100g of petroleum ether into the reactor, then add 228g of triethylamine, and then add 120g of vinyltrichlorosilane dropwise at 60°C under stirring and normal pressure for 3 hours. After the addition is completed, continue to keep warm for 3h. After the addition is completed, stand and separate the layers, separate the triethylamine hydrochloride layer, and distill the crude product at the upper layer. Distill at a distillation temperature of 100°C and a distillation pressure of 750mmHg to obtain the product ethyl lactate silane. 286 kg of product was obtained with a yield of 94.6% (based on chlorosilane). The reaction product test results showed that the purity of vinyl triethyl lactate silane was 92.5%, the content of ethyl lactate was 1.50%, the color APHA was 100, and the chloride ion was 10 ppm. Alkaline water containing 35 kg of caustic soda flakes and 142 kg of water was added to triethylamine hydrochloride, and the mixture was stirred for neutralization, layered, and dehydrated to recover triethylamine. The mixture contained 51 kg of sodium chloride and 192 kg of trace triethylamine waste water, and the water consumption was equivalent to 0.5 ton / ton of product.
[0039] Comparative Example 3: Compared with Example 1, the pore size of the membrane in Comparative Example 3 is too large, and the pore size of the membrane is 5 μm.
[0040] Comparative Example 4: Compared with Example 1, the pore size of the membrane in Comparative Example 4 is too small, and the pore size of the membrane is 0.01 μm.
[0041] Test example: The product quality, production efficiency and water consumption of wastewater treatment per ton of product obtained when producing ethyl lactate silane products in Examples 1 to 3 and Comparative Examples 1 to 4 were statistically analyzed. The product quality includes the purity of ethyl lactate silane and the content of ethyl lactate, chromaticity and chloride ions. The production efficiency includes the daily production capacity and the material conversion rate based on silane. The statistical results are shown in Table 1. Table 1 Statistical results As shown in Table 1, Examples 1 to 6 are production data and product data of ethyl lactate silane produced by the method for preparing ethyl lactate silane and the reaction device of the present invention. The results show that the purity of ethyl lactate silane is 95.8-98.2%, the content of ethyl lactate in the product is 0.52-0.18%, the chroma is 5-10, and the chloride ion content of the product is 1-4ppm. The results show that the ethyl lactate product prepared by the present invention has a high conversion rate, low chroma, less impurity content in the product, high product conversion rate, and significantly improved product quality; in addition, the daily production capacity of the present invention is 7000-8720Kg, the yield of the material based on chlorosilane is 99.4-99.8%, and no wastewater treatment is required per ton of product, and the water consumption is zero.
[0042] Comparative Example 1 is a production process for the direct reaction of vinyltrichlorosilane and ethyl lactate. The results show that the purity of the ethyl lactate silane in Comparative Example 1 is 94.8%, the ethyl lactate content in the product is 1.78%, the chromaticity is 50, the chloride ion content in the product is 15, the daily production capacity is 1320Kg, the material yield based on chlorosilane is 96.2%, and 0.68 tons / ton of acid-containing wastewater will be generated, which is equivalent to 0.51 tons / ton of water consumption. Compared with Examples 1 to 6, Comparative Example 1 has high product chromaticity, high impurity content and low product quality. In addition, the production capacity of Comparative Example 1 is significantly lower than that of the present invention and a large amount of acid-containing wastewater will be generated, the production energy consumption is high and the production efficiency is low.
[0043] Comparative Example 2 is a production process using triethylamine acid binding agent. The results show that the purity of the ethyl lactate silane of Comparative Example 1 of Comparative Example 2 is 92.5%, the ethyl lactate content in the product is 1.5%, the chromaticity is 100, the chloride ion content in the product is 10, the daily production capacity is 980Kg, the material yield based on chlorosilane is 94.6%, and 0.67 tons of waste water containing ammonium chloride and triethylamine will be generated, which is equivalent to 0.5 tons of water consumption per ton of product. Compared with Examples 1 to 6, Comparative Example 2 has high product chromaticity, high impurity content and low product quality. In addition, the production capacity of Comparative Example 2 is significantly lower than that of the present invention and a large amount of acid-containing waste water will be generated, the production energy consumption is high and the production efficiency is low.
[0044] Comparative Examples 3 and 4 tested the technical solutions of membrane pore size being too large and too small respectively. The results showed that if the pore size of the membrane is too large, the liquid will not be able to pass through the membrane for application, while if the pore size of the membrane is too small, ammonia cannot enter the membrane for neutralization reaction, the side reactions of the reaction products increase, the impurities in the products increase, the purity of the products decreases significantly, and effective production cannot be carried out.
[0045] The above description is only a preferred embodiment of the present invention and does not limit the present invention in any way. Any simple modification, change and equivalent transformation made to the above embodiment based on the technical essence of the present invention still falls within the protection scope of the technical solution of the present invention.
Claims
1. A method for preparing ethyl lactate silane, characterized in that: The following steps are involved: Ammonia gas is introduced into the shell, solvent oil, ethyl lactate and chlorosilane are injected into the membrane reaction component in the shell to react to produce a crude product, and the crude product is filtered and distilled to produce ethyl lactate silane; the membrane reaction unit includes a hollow frame and a membrane arranged on the hollow frame, and the pore size of the membrane is 0.1~1 μm.
2. The preparation method according to claim 1, characterized in that: The mass ratio of solvent oil to chlorosilane is 3-8:1, and the molar ratio of ethyl lactate to chlorine in chlorosilane is 1-1.01:
1.
3. The preparation method according to claim 1, characterized in that: The pressure of the ammonia gas is 100-200 Kpa, the reaction temperature is 30-60° C., and the pH of the crude product is 7-13.
4. The preparation method according to claim 1 or 2, characterized in that: The chlorosilane is one or more of methyltrichlorosilane, vinyltrichlorosilane, phenyltrichlorosilane or silicon tetrachloride.
5. A reaction device, characterized in that: The invention comprises a shell (1) and a membrane reaction component (2) arranged in the shell, wherein the membrane reaction component comprises a plurality of membrane reaction units (201) connected to each other, and the shell and the membrane reaction component are the shell and the membrane reaction component in the method for preparing ethyl lactate silane according to any one of claims 1 to 4.
6. The reaction device according to claim 5, characterized in that: The membrane reaction unit comprises a hollow frame (211) and a membrane (212) arranged on the hollow frame, windows (213) are arranged on both side surfaces of the hollow frame, the membrane is detachably connected to the window, a card slot is arranged on the window, a support frame is arranged on the outer edge of the membrane, and a buckle detachably connected to the card slot is arranged on the support frame.
7. The reaction device according to claim 5 or 6, characterized in that: The spacing between membranes in the membrane reaction unit is 1-5 mm, the spacing between the membrane reaction units is 50-200 mm, the width of the membrane reaction unit is 5-200 mm, and the aspect ratio of the membrane reaction unit is greater than 2.
8. The reaction device according to claim 5, characterized in that: The shell is provided with an air inlet (101), a liquid inlet (103) and a liquid outlet (104); the liquid outlet is provided with a pH detection device (105); the liquid outlet is connected to a filtering and distilling device; the liquid inlet is connected to a chlorosilane feeder (109), a lactate feeder (110) and a heat exchange device (107); the heat exchange device is connected to an oil solvent feeder (108); and a temperature tester (111) and a pressure tester (112) are provided inside the shell.
9. The reaction device according to claim 8, characterized in that: The filtering and distilling device comprises a tank body and a filter screen arranged in the tank body.
10. The reaction device according to claim 9, characterized in that: The filter screen is provided with a scraper.