A production device for continuously synthesizing tetraethyl orthosilicate

Abstract

The utility model discloses a kind of production device for continuous synthesis tetraethyl orthosilicate, including the microchannel reaction device first module, first gas-liquid separation device, microchannel reaction device second module, second gas-liquid separation device, storage tank, tail gas absorption tank, first plunger pump, second plunger pump, third plunger pump and fourth plunger pump connected in sequence.The utility model uses segmented microchannel reaction device design, carries out fractional esterification.Microchannel design effectively improves reaction efficiency under the condition of reducing reaction temperature.

Description

Technical Field

[0001] This utility model relates to the field of chemical production equipment technology, and more specifically, it relates to a production apparatus for the continuous synthesis of tetraethyl orthosilicate. Background Technology

[0002] Tetraethyl orthosilicate is an organosilicon compound widely used in industry, primarily as a coating, waterproofing material, adhesive, and refractory material. In recent years, tetraethyl orthosilicate has attracted significant attention as a commonly used precursor in the synthesis of new materials, particularly in the fields of semiconductors, photovoltaics, and high-purity silica sand.

[0003] Currently, the synthesis of tetraethyl orthosilicate in the industry mostly involves a batch reaction using silicon tetrachloride and ethanol as raw materials. This process suffers from drawbacks such as intense exothermic reaction, low conversion rate, numerous byproducts, and low production efficiency. In recent years, microreactors, due to their strong heat exchange and mass transfer characteristics, have been widely used in various organic reactions, especially highly exothermic and hazardous reactions, significantly improving reaction temperature control, shortening reaction time, and increasing reaction selectivity. However, because this reaction process generates a large amount of hydrogen chloride gas, failure to promptly remove it can inhibit the forward esterification reaction. Therefore, it is difficult to achieve efficient synthesis of tetraethyl orthosilicate using only microreactors, and a large amount of byproducts such as triethoxychlorosilane still exist. To address these issues, a continuous synthesis device for tetraethyl orthosilicate was designed. Utility Model Content

[0004] (a) Technical problems to be solved

[0005] In view of the problems existing in the prior art, this utility model provides a production apparatus for continuous synthesis of tetraethyl orthosilicate to solve the technical problems mentioned in the background art.

[0006] (II) Technical Solution

[0007] To achieve the above objectives, the present invention provides the following technical solution: a production apparatus for continuous synthesis of tetraethyl orthosilicate, comprising a first module of a microchannel reaction device, a first gas-liquid separation device, a second module of a microchannel reaction device, a second gas-liquid separation device, a storage tank, a tail gas absorption tank, a first plunger pump, a second plunger pump, a third plunger pump, and a fourth plunger pump connected in sequence.

[0008] The present invention is further configured such that the reaction temperature of the first module of the reaction device is 30-60 degrees Celsius.

[0009] The present invention is further configured such that the reaction temperature of the second module of the microchannel reaction device is 30-60 degrees Celsius.

[0010] The present invention is further configured such that the reaction time of the first module of the reaction device is 10-60s.

[0011] The present invention is further configured such that the reaction time of the second module of the microchannel reaction device is 10-30s.

[0012] (III) Beneficial Effects

[0013] Compared with the prior art, this utility model provides a production apparatus for the continuous synthesis of tetraethyl orthosilicate, which has the following beneficial effects:

[0014] This invention employs a segmented microchannel reaction device design for stepwise esterification. The microchannel design effectively improves reaction efficiency while lowering the reaction temperature. During the synthesis of tetraethyl orthosilicate, a large amount of hydrogen chloride gas is generated, inhibiting the conversion of triethoxychlorosilane to tetraethyl orthosilicate. The design of adding a gas-liquid separator after the microchannel reaction device removes the large amount of hydrogen chloride gas generated in the first stage of esterification, effectively improving the rate and conversion of the second stage esterification reaction. Excess hydrogen chloride gas reacts with ethanol, increasing the molar amount of ethanol required. Timely removal of hydrogen chloride gas effectively reduces the molar amount of ethanol required, preventing subsequent corrosion of the equipment by the hydrogen chloride gas. Attached Figure Description

[0015] Figure 1 This is a schematic diagram of the overall structure of a production apparatus for the continuous synthesis of tetraethyl orthosilicate according to the present invention.

[0016] In the figure: 1. First module of microchannel reaction device; 2. First gas-liquid separation device; 3. Second module of microchannel reaction device; 4. Second gas-liquid separation device; 5. Storage tank; 6. Tail gas absorption tank; 7. First plunger pump; 8. First plunger pump; 9. First plunger pump; 10. First plunger pump. Detailed Implementation

[0017] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.

[0018] It should be noted that, unless otherwise specified, all technical and scientific terms used in this application have the same meaning as commonly understood by one of ordinary skill in the art to which this application pertains.

[0019] In this utility model, unless otherwise stated, the orientations used, such as "up" and "down", usually refer to the direction shown in the accompanying drawings, or to the vertical, perpendicular, or gravitational direction; similarly, for ease of understanding and description, "left" and "right" usually refer to the left and right shown in the accompanying drawings; "inner" and "outer" refer to the inner and outer contours of each component itself, but the above directional terms are not used to limit this utility model.

[0020] Please see Figure 1 A production apparatus for the continuous synthesis of tetraethyl orthosilicate includes a first module of a microchannel reaction device, a first gas-liquid separation device, a second module of a microchannel reaction device, a second gas-liquid separation device, a storage tank, a tail gas absorption tank, a first plunger pump, a second plunger pump, a third plunger pump, and a fourth plunger pump connected in sequence.

[0021] In a further embodiment of this utility model, the reaction temperature of the first module of the reaction device is 30-60 degrees Celsius; the reaction temperature of the second module of the microchannel reaction device is 30-60 degrees Celsius; the reaction time of the first module of the reaction device is 10-60 seconds; and the reaction time of the second module of the microchannel reaction device is 10-30 seconds.

[0022] In the synthesis of tetraethyl orthosilicate, silicon tetrachloride and ethanol are continuously fed by a first plunger pump 7 and a second plunger pump 8 at a molar ratio of 1:(3.00 to 3.05). The first stage of esterification reaction is carried out in the first reaction module 1 of the microchannel reactor with a residence time of 10 to 60 s and a heat exchange temperature of 30 to 60 °C. Triethoxychlorosilane and small amounts of monoethoxytrichlorosilane, diethoxydichlorosilane and tetraethyl orthosilicate are generated. The reaction liquid is transported to the first gas-liquid separator 2 to separate hydrogen chloride gas, which is then discharged into the tail gas absorption tank 6. The reaction liquid enters the second reaction module 3 of the microchannel reactor via the third plunger pump 9. Simultaneously, ethanol is continuously fed through the fourth plunger pump 10 at a molar ratio of silicon tetrachloride to ethanol of 1:(1.00 to 1.05). The residence time in the second reaction module 3 of the microchannel reactor is 10-30 seconds, and the heat exchange temperature of the second reaction module 3 of the microchannel reactor is 30 to 60°C. The reaction liquid is then transported to the second gas-liquid separator 4 to separate hydrogen chloride gas, and finally transported to the storage tank 5. The yield is not less than 99.0%.

[0023] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A production apparatus for the continuous synthesis of tetraethyl orthosilicate, characterized in that, It includes a microchannel reaction device first module, a first gas-liquid separation device, a microchannel reaction device second module, a second gas-liquid separation device, a storage tank, a tail gas absorption tank, a first plunger pump, a second plunger pump, a third plunger pump, and a fourth plunger pump connected in sequence.

2. The production apparatus for continuous synthesis of tetraethyl orthosilicate according to claim 1, characterized in that: The reaction temperature of the first module of the reaction device is 30-60 degrees Celsius.

3. The production apparatus for continuous synthesis of tetraethyl orthosilicate according to claim 1, characterized in that: The reaction temperature of the second module of the microchannel reaction device is 30-60 degrees Celsius.

4. The production apparatus for continuous synthesis of tetraethyl orthosilicate according to claim 1, characterized in that: The reaction time of the second module of the microchannel reaction device is 10-30 seconds.

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