A continuous tower alcoholysis system and method for high boiling chlorosilanes

By designing a continuous tower-type alcoholysis system for high-boiling-point chlorosilanes, employing vacuum vaporization and washing distillation processes, and using zirconium equipment and metal zirconium gaskets for sealing, the problems of equipment blockage and easy damage during the alcoholysis of high-boiling-point chlorosilanes were solved, achieving stable and efficient alcoholysis results.

CN117205854BActive Publication Date: 2026-05-08ZHEJIANG KAIHUA SYNTHETIC MATERIAL
View PDF 1 Cites 0 Cited by

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
ZHEJIANG KAIHUA SYNTHETIC MATERIAL
Filing Date
2023-09-11
Publication Date
2026-05-08

AI Technical Summary

Technical Problem

Existing technologies cannot effectively handle the alcoholysis process of high-boiling-point chlorosilanes, leading to equipment blockage, low efficiency, and easy damage and high maintenance costs, which cannot meet the long-term stable operation requirements of high-boiling-point chlorosilanes.

Method used

A continuous tower-type alcoholysis system for high-boiling-point chlorosilanes is designed, including an alcohol pretreatment unit, a chlorosilane pretreatment unit, an alcoholysis unit, and an alcoholysis gas product processing unit. The system employs vacuum vaporization and washing distillation processes to remove iron impurities and uses zirconium equipment and metallic zirconium gaskets for sealing to ensure the stable conduction of the alcoholysis reaction.

Benefits of technology

It achieves stable and efficient alcoholysis of high-boiling-point chlorosilanes, reduces equipment maintenance costs, improves equipment durability and ease of operation, has a wide range of applications, and is suitable for the long-term stable operation of high-boiling-point chlorosilanes.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN117205854B_ABST
    Figure CN117205854B_ABST
Patent Text Reader

Abstract

The application provides a continuous tower type alcoholysis system and method of high-boiling chlorosilane, comprising: an alcohol pretreatment unit comprising an alcohol vaporizer, a demister, an alcohol superheater and a falling film reboiler connected in sequence; a chlorosilane pretreatment unit comprising a falling film evaporator, a settling separator, a washing tower and a stripping tower; and an alcoholysis unit comprising an alcoholysis tower, a neutralization tank and a crude esterification product storage tank connected in sequence, wherein the pretreated alcohol vapor is introduced from the lower part of the alcoholysis tower, the pretreated chlorosilane liquid is introduced from the upper part of the alcoholysis tower, and the obtained liquid material is discharged from the bottom of the alcoholysis tower into the neutralization tank after the alcoholysis reaction, and then is discharged into the crude esterification product storage tank after neutralization with sodium alcoholate in the neutralization tank. The continuous tower type alcoholysis system and method of high-boiling chlorosilane have the advantages of simple structure, convenient operation, wide application range, safety and high efficiency, and long-term stable operation.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of organosilicon technology, and in particular to a continuous tower-type alcoholysis system and method for high-boiling-point chlorosilanes. Background Technology

[0002] In the production of organosilicon products, high-boiling-point chlorosilanes with two or more chlorine atoms attached to their silicon atoms are prone to cross-linking and solidification reactions when reacting with alcohols to form alkoxysilanes. This can cause equipment blockage. If these chlorosilanes cannot be converted and utilized through low-cost alcoholysis and are instead allowed to accumulate in large quantities within the chemical plant, it will seriously affect efficiency and safety. Furthermore, for high-boiling-point specialty chlorosilane monomers, such as phenylchlorosilanes and long-chain alkane-based chlorosilanes, a low-cost continuous tower alcoholysis esterification process is also required to improve yield and purity.

[0003] However, due to the steric hindrance of the molecular structure of high-boiling-point chlorosilanes, their reaction with alcohols requires higher reaction temperatures and longer reaction times to be complete. Increasing the reaction temperature accelerates the reaction of alcohols with hydrogen chloride to produce chloroalkanes and water. Water readily undergoes cross-linking and curing reactions with these chlorosilanes, leading to equipment blockage. Furthermore, when the raw materials contain iron impurities or equipment factors cause the raw materials to come into contact with ferric chloride, ferric chloride has a strong catalytic effect, enabling the alcohol to react with hydrogen chloride to produce chloroalkanes and water, making the cross-linking and curing reaction more likely to occur. When using a continuous alcoholysis process to process high-boiling-point chlorosilanes on a large scale, if the reaction temperature is low and a tower reaction process using alcohol vapor stripping to remove acid is employed under atmospheric or pressurized conditions, the vapor pressure of the high-boiling-point chlorosilanes in the liquid phase and the mixture of alkoxysilanes obtained from partial alcoholysis is very low, resulting in strong saturation solubility. This allows alcohols and hydrogen chloride to easily dissolve simultaneously and in large quantities in the liquid phase. The presence of iron impurities in the liquid phase catalyzes the formation of water, easily leading to the cross-linking and curing reaction. However, the current continuous tower reaction method does not remove iron from the raw materials, nor does it have measures to prevent high-boiling-point chlorosilanes from causing solidification blockage in the refrigeration equipment of the hydrogen chloride separation system. Therefore, it cannot handle high-boiling-point chlorosilanes.

[0004] Furthermore, most existing processes utilize enamel- or glass-lined tower equipment to complete the alcoholysis reaction of chlorosilanes. This equipment has numerous tower sections and sealing surfaces, making it susceptible to damage from vibration and impact. The tower sections are typically sealed with PTFE-coated gaskets, which are prone to deformation and failure at high temperatures, leading to frequent gasket replacements. More seriously, frequent shutdowns for gasket replacement expose the material to the atmosphere, causing severe corrosion and damage to the equipment, increasing maintenance costs. Additionally, the height of enamel- and glass-lined towers is limited by the corrosion protection layer and the allowable strength of the gaskets. Using a single tower makes it difficult to meet the residence time required for the alcoholysis reaction of high-boiling-point chlorosilanes. However, using multiple towers in series creates localized acid removal problems, complicating the system structure and operation. Moreover, the heating and cooling of enamel- and glass-lined equipment must be slow, as thermal stress caused by temperature fluctuations can easily damage the corrosion protection layer, making high-temperature operation difficult.

[0005] In the current context of the booming development of organosilicon industry in my country, it is of great significance to provide a continuous tower alcoholysis system and method for high-boiling-point chlorosilanes, which enables the long-term stable and efficient operation of the chlorosilane alcoholysis process. Summary of the Invention

[0006] This invention designs a continuous tower-type alcoholysis system and method for high-boiling-point chlorosilanes to achieve long-term stable and efficient operation of the chlorosilane alcoholysis process.

[0007] To address the above problems, this invention discloses a continuous tower-type alcoholysis system for high-boiling-point chlorosilanes, comprising:

[0008] The alcohol pretreatment unit includes an alcohol vaporizer, a demister, an alcohol superheater, and a falling film reboiler connected in sequence. After the alcohol raw material is vaporized by the alcohol vaporizer, it is passed into the demister for demisting treatment, and then passed into the alcohol superheater and the falling film reboiler for heating treatment to obtain pretreated alcohol vapor.

[0009] The chlorosilane pretreatment unit includes a falling film evaporator, a settling separator, a washing tower, and a stripping tower. The chlorosilane raw material is first fed into the falling film evaporator and heated to vaporize. The unvaporized liquid is discharged into the settling separator. After impurities are removed by the settling separator, the steam is discharged into the washing tower. After washing and purification in the washing tower, it is fed into the stripping tower to remove light components, thus obtaining the pretreated chlorosilane.

[0010] The alcoholysis unit includes an alcoholysis tower, a neutralization tank, and a crude esterification product storage tank connected in sequence. Pretreated alcohol vapor is introduced from the bottom of the alcoholysis tower, and pretreated chlorosilane vapor is introduced from the top of the alcoholysis tower. After the two undergo alcoholysis reaction in the alcoholysis tower, the resulting liquid material is discharged from the bottom of the alcoholysis tower into the neutralization tank. After neutralization with sodium alkoxide in the neutralization tank, it is discharged into the crude esterification product storage tank.

[0011] Furthermore, some of the chlorosilanes purified by the settling separator are returned to the falling film evaporator; the remaining chlorosilane vapors are fed into the scrubbing tower for washing and purification.

[0012] The clean chlorosilane discharged from the top of the washing tower is fed into the stripping tower for further processing, while the material discharged from the bottom of the washing tower is returned to the falling film evaporator and, together with the material from the chlorosilane raw material storage tank, enters the falling film evaporator for processing.

[0013] Furthermore, an iron-removed chlorosilane storage tank is provided at the bottom of the stripping tower, which stores iron-removed chlorosilane. A portion of the material in the iron-removed chlorosilane storage tank is sent to the top of the alcoholysis tower for alcoholysis reaction, and another portion of the material is sent to the top of the washing tower to wash the gaseous material inside.

[0014] Furthermore, the continuous column alcoholysis system for high-boiling-point chlorosilanes also includes:

[0015] The alcoholysis gas product processing unit includes a vacuum pump, a dechlorinated silane tower, and a hydrogen chloride purification tower. The alcoholysis gas product discharged from the top of the alcoholysis tower is first introduced into the top of the stripping tower, and then drawn into the dechlorinated silane tower by the vacuum pump. After being processed by the dechlorinated silane tower, it is discharged into the hydrogen chloride purification tower.

[0016] Furthermore, part of the material from the chlorosilane storage tank enters the falling film evaporator, while another part enters the vacuum pump. After mixing with the alcoholysis gas products from the stripping tower, the mixture is discharged into the lower part of the dechlorinated silane tower via the vacuum pump. After being distilled in the dechlorinated silane tower, the gas is discharged from the upper part of the dechlorinated silane tower into the hydrogen chloride purification tower; the liquid is discharged from the lower part of the dechlorinated silane tower into the falling film evaporator.

[0017] Furthermore, the alcoholysis tower includes an upper alcoholysis tower and a lower alcoholysis tower, wherein the bottom of the upper alcoholysis tower is connected to the upper part of the lower alcoholysis tower, alcohol vapor from the alcohol pretreatment unit is introduced into the lower part of the lower alcoholysis tower, and chlorosilane from the chlorosilane pretreatment unit is introduced into the upper part of the upper alcoholysis tower. During the alcoholysis reaction, the material at the bottom of the upper alcoholysis tower is introduced into the lower alcoholysis tower to continue the reaction, and the material from the top of the lower alcoholysis tower is introduced into the lower part of the upper alcoholysis tower to continue the reaction. The bottom of the lower alcoholysis tower is connected to the neutralization tank, and the liquid material discharged from the bottom of the lower alcoholysis tower is further processed in the neutralization tank. The alcoholysis gaseous product discharged from the top of the upper alcoholysis tower enters the alcoholysis gaseous product processing unit for processing.

[0018] Furthermore, the alcoholysis gas product processing unit includes: a dechlorinated silane lower column, a vacuum pump, a dechlorinated silane upper column, a membrane compressor, and a hydrogen chloride purification column. The alcoholysis gas product discharged from the upper part of the alcoholysis column is first introduced into the upper part of the stripping column, then passes through the alcohol vaporizer and enters the dechlorinated silane lower column. After rectification treatment in the dechlorinated silane lower column, the gas is pumped from the top of the dechlorinated silane lower column to the lower part of the dechlorinated silane upper column by the vacuum pump. The material discharged from the bottom of the dechlorinated silane lower column is introduced into the falling film evaporator. After the material is rectified again in the dechlorinated silane upper column, the generated gas is discharged from the top of the dechlorinated silane upper column and enters the membrane compressor. After being compressed by the membrane compressor, it is introduced into the hydrogen chloride purification column for rectification treatment. The liquid material at the bottom of the dechlorinated silane upper column is introduced into the upper part of the dechlorinated silane lower column.

[0019] Furthermore, the alcoholysis tower includes a zirconium metal alcoholysis tower and an enamel-lined alcoholysis tower, wherein the bottom of the enamel-lined alcoholysis tower is connected to the top of the zirconium metal alcoholysis tower. Alcohol vapor from the alcohol pretreatment unit is introduced into the bottom of the zirconium metal alcoholysis tower, and chlorosilane from the chlorosilane pretreatment unit is introduced into the top of the enamel-lined alcoholysis tower. During the alcoholysis reaction, the material at the bottom of the enamel-lined alcoholysis tower is introduced into the zirconium metal alcoholysis tower for further reaction, and the material at the top of the zirconium metal alcoholysis tower is introduced into the enamel-lined alcoholysis tower for further reaction. The bottom of the zirconium metal alcoholysis tower is connected to the neutralization tank. The liquid material discharged from the bottom of the zirconium metal alcoholysis tower is further processed in the neutralization tank, and the alcoholysis gaseous product discharged from the top of the enamel-lined alcoholysis tower enters the alcoholysis gaseous product processing unit for processing.

[0020] Furthermore, the alcohol vaporizer, falling film reboiler, and stripping tower are made of zirconium, while the demister, alcohol superheater, and washing tower are made of pure nickel.

[0021] A continuous column alcoholysis method for high-boiling-point chlorosilanes, wherein the method employs the aforementioned continuous column alcoholysis system for the alcoholysis of chlorosilanes.

[0022] The continuous tower alcoholysis system and method for high-boiling-point chlorosilanes described in this application have the advantages of simple structure, convenient operation, wide applicability, safety and efficiency, and long-term stable operation. Attached Figure Description

[0023] Figure 1 This is a process flow diagram of the continuous tower alcoholysis system for high-boiling-point chlorosilanes described in Example 1 of the present invention;

[0024] Figure 2 This is a process flow diagram of the continuous tower alcoholysis system for high-boiling-point chlorosilanes described in Example 2 of the present invention;

[0025] Figure 3 This is a process flow diagram of the continuous tower alcoholysis system for high-boiling-point chlorosilanes described in Example 3 of the present invention;

[0026] Figure 4 This is a schematic diagram of the auxiliary system of the alcohol vaporizer described in Embodiment 4 of the present invention;

[0027] Figure 5 This is a schematic diagram of the auxiliary system of the falling film evaporator described in Embodiment 5 of the present invention. Detailed Implementation

[0028] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

[0029] Example 1

[0030] like Figure 1 As shown, a continuous tower-type alcoholysis system for high-boiling-point chlorosilanes includes:

[0031] The alcohol pretreatment unit includes an alcohol vaporizer, a demister, an alcohol superheater, and a falling film reboiler connected in sequence. After the alcohol raw material is vaporized by the alcohol vaporizer, it is passed into the demister for demisting treatment, and then passed into the alcohol superheater and the falling film reboiler for heating treatment to obtain pretreated alcohol vapor.

[0032] The chlorosilane pretreatment unit includes a falling film evaporator, a settling separator, a washing tower, and a stripping tower. The chlorosilane raw material is first fed into the falling film evaporator and heated to vaporize. The unvaporized liquid is discharged into the settling separator. After impurities are removed by the settling separator, the steam is discharged into the washing tower. After washing and purification in the washing tower, it is fed into the stripping tower to remove light components, thus obtaining the pretreated chlorosilane.

[0033] The alcoholysis unit includes an alcoholysis tower, a neutralization tank, and a crude esterification product storage tank connected in sequence. Pretreated alcohol vapor is introduced from the bottom of the alcoholysis tower, and pretreated chlorosilane liquid is introduced from the top of the alcoholysis tower. After the two undergo alcoholysis reaction in the alcoholysis tower, the resulting liquid material is discharged from the bottom of the alcoholysis tower into the neutralization tank. After neutralization with sodium alkoxide in the neutralization tank, it is discharged into the crude esterification product storage tank.

[0034] Furthermore, the alcohol pretreatment unit also includes:

[0035] An alcohol raw material tank, which stores alcohol raw materials;

[0036] Pump 3, located between the alcohol feedstock tank and the alcohol vaporizer, is used to pump the alcohol feedstock in the alcohol feedstock tank to the alcohol vaporizer for heating and vaporization.

[0037] Furthermore, in the alcohol pretreatment unit:

[0038] The liquid inlet of the alcohol vaporizer is connected to the alcohol raw material tank, and the gas outlet of the alcohol vaporizer is connected to the material inlet of the demister, so that the alcohol raw material in the alcohol raw material tank can be pumped to the alcohol vaporizer by the pump 3, and vaporized in the alcohol vaporizer before entering the demister;

[0039] The material outlet of the demister is connected to the material inlet of the alcohol superheater, the material outlet of the alcohol superheater is connected to the material inlet of the falling film reboiler, and the material outlet of the falling film reboiler is connected to the lower part of the alcoholysis tower. The alcohol vapor after being demisted by the demister first enters the alcohol superheater, and after being heated by the alcohol superheater, it enters the falling film reboiler, mixes with the reflux liquid in the falling film reboiler, and then enters the lower part of the alcoholysis tower.

[0040] Furthermore, the chlorosilane pretreatment unit also includes:

[0041] A chlorosilane raw material storage tank, which stores chlorosilane raw materials;

[0042] Pump 4, located between the chlorosilane raw material storage tank and the falling film evaporator, is used to pump the stored chlorosilane raw material in the chlorosilane raw material storage tank into the falling film evaporator.

[0043] Furthermore, a pump 2 is installed between the falling film evaporator and the sedimentation separator. The material inlet of the pump 2 is connected to the clean material outlet of the sedimentation separator, so as to pump and return a portion of the clean material processed by the sedimentation separator to the falling film evaporator.

[0044] As some embodiments of this application, the chlorosilane pretreatment unit further includes a slag discharge system, the material inlet of which is connected to the slag discharge port of the settling separator, for treating the solid impurities discharged from the settling separator. Preferably, the settling separator is an intermittent slag discharge system, and the slag discharge system is periodically activated to treat the solid impurities.

[0045] Preferably, some of the chlorosilanes purified by the settling separator are returned to the falling film evaporator via the pump 2; the remaining chlorosilane vapors are fed into the washing tower for washing and purification.

[0046] Furthermore, an iron-removed chlorosilane storage tank is provided at the lower part of the stripping tower, which stores the iron-removed chlorosilane. The inlet of the iron-removed chlorosilane storage tank is connected to the lower part of the stripping tower, and the outlet is connected to the upper part of the washing tower through pump 5.

[0047] During operation, a portion of the material in the iron-removed chlorosilane storage tank is pumped to the upper part of the alcoholysis tower via pump 5, and another portion is pumped to the upper part of the washing tower via pump 5. The chlorosilane from the settling separator is then washed and purified by spraying downwards from the upper part of the washing tower. The clean chlorosilane discharged from the top of the washing tower is fed into the stripping tower for further processing, while the material discharged from the bottom of the washing tower is returned to the falling film evaporator and, together with the material from the chlorosilane raw material storage tank, enters the falling film evaporator for further processing.

[0048] Furthermore, the alcoholysis unit also includes:

[0049] A sodium alkoxide feeding tank, connected to the neutralization tank, is used to inject sodium alkoxide into the neutralization tank;

[0050] Pump 1, located between the alcoholysis tower and the neutralization tank, is used to pump the liquid material at the bottom of the alcoholysis tower into the neutralization tank for neutralization reaction with sodium alkoxide.

[0051] As some embodiments of this application, the bottom of the alcoholysis tower is also connected to the falling film reboiler, which is used to return part of the material discharged from the alcoholysis tower to the falling film reboiler, and mix it with the alcohol vapor in the falling film reboiler before passing it back into the lower part of the alcoholysis tower. In this way, alcohol vapor and chlorosilanes and other substances can undergo pre-reaction in the falling film reboiler before entering the alcoholysis tower, thereby improving the degree of reaction.

[0052] As some embodiments of this application, the neutralization tank can be one or multiple tanks arranged in parallel, such as neutralization tank 1, neutralization tank 2 and neutralization tank 3 arranged in parallel.

[0053] Specifically, in actual operation, the product yield and purity can be adjusted by the reflux ratio of the material in the neutralization tank back to the falling film reboiler.

[0054] In addition, the continuous tower alcoholysis system for high-boiling-point chlorosilanes also includes:

[0055] The alcoholysis gas product processing unit includes a vacuum pump, a dechlorinated silane tower, and a hydrogen chloride purification tower. The alcoholysis gas product discharged from the top of the alcoholysis tower is first introduced into the top of the stripping tower, and then drawn into the dechlorinated silane tower by the vacuum pump. After being processed by the dechlorinated silane tower, it is discharged into the hydrogen chloride purification tower.

[0056] Preferably, the alcohol vaporizer is connected to the top of the stripping tower, and the alcoholysis gas products introduced into the stripping tower can enter the alcohol vaporizer from the top, exchange heat with the alcohol feedstock in the alcohol vaporizer, and then enter the vacuum pump.

[0057] As some embodiments of the present invention, the vacuum pump is a magnetically driven liquid ring vacuum pump.

[0058] As some embodiments of the present invention, part of the material from the chlorosilane storage tank enters the falling film evaporator through pump 4, and another part of the material enters the vacuum pump. After mixing with the alcoholysis gas products from the stripping tower, the mixture is discharged into the lower part of the dechlorination silane tower through the vacuum pump. After being distilled by the dechlorination silane tower, the gas is discharged from the upper part of the dechlorination silane tower into the hydrogen chloride purification tower; the liquid is discharged from the lower part of the dechlorination silane tower into the falling film evaporator.

[0059] Furthermore, the alcoholysis gas product processing unit also includes a saturated hydrocarbon feed tank, which stores saturated hydrocarbons. The saturated hydrocarbon feed tank is connected to the dechlorination silane tower and is used to replenish a certain amount of saturated hydrocarbons into the dechlorination silane tower when needed.

[0060] Furthermore, a refrigeration condenser is installed at the top of the hydrogen chloride purification tower, and a reboiler and a cooler are installed at the bottom. The material discharged from the dechlorinated silane tower is distilled in the hydrogen chloride purification tower, and the gas is discharged from the top of the hydrogen chloride purification tower into the refrigeration condenser. After being processed by the refrigeration condenser, it can be supplied as clean hydrogen chloride gas to hydrogen chloride users. The material discharged from the bottom of the hydrogen chloride purification tower enters the reboiler. After being heated by the reboiler, the gaseous material enters the hydrogen chloride purification tower, and the liquid material is discharged to the cooler for cooling.

[0061] Furthermore, the alcoholysis gas product processing unit further includes:

[0062] A chloroalkane tower, connected to the cooler, is used to distill the material discharged from the cooler.

[0063] Pump 7, which is disposed between the cooler and the chloroalkane tower, is used to pump the material in the cooler into the chloroalkane tower;

[0064] And a chloroalkane storage tank, which is connected to the top of the chloroalkane tower for collecting material discharged from the top of the chloroalkane tower.

[0065] Furthermore, the bottom of the chloroalkane tower is connected to the top of the dechlorinated silane tower, and the material discharged from the bottom of the chloroalkane tower is circulated into the top of the dechlorinated silane tower for further processing.

[0066] This invention employs a process of vacuum vaporization and washing distillation of raw materials to remove iron impurities, copper impurities, and fluoride ions carried by the reaction raw materials, prevents alcohol and hydrogen chloride from reacting catalyzed in the alcoholysis tower to generate water, and inhibits the generation of cross-linking and solidification reactions.

[0067] The vacuum treatment process can lower the boiling point temperature of the material, prevent the raw material chlorosilane from decomposing and deteriorating due to excessively high temperature during vaporization, and make the ferric chloride solidify and be easily washed and separated.

[0068] Furthermore, this invention utilizes thermal energy in stages to reduce energy consumption. Specifically, the vaporization pressure of the alcohol is controlled so that the vaporization temperature of the alcohol is higher than the solidification temperature of the chlorosilane to prevent chlorosilane from clogging the equipment; a stripping tower is used to ensure that the temperature of the condensed chlorosilane liquid meets the feed requirements of the alcoholysis tower; the selected alcohol vaporizer is a vertical falling film evaporator, and the flow resistance between the alcoholysis products and the pipes is reduced.

[0069] Preferably, the alcohol vaporizer, falling film reboiler, stripping tower and iron-removed chlorosilane tank can be made of zirconium, while the demister, alcohol superheater and scrubbing tower can be made of pure nickel.

[0070] More preferably, because the tower body lined with zirconium or tantalum is difficult to manufacture and is prone to generating harmful thermal stress, which is not conducive to high-temperature operation, and poor manufacturing process can cause the lining to fall off easily under vacuum, this embodiment selects a reaction tower with a high zirconium metal single tower as the alcoholysis tower.

[0071] The alcoholysis column is constructed into multiple sections, which are connected by loose carbon steel flanges for secure fastening. Zirconium or tantalum gaskets are used on the sealing surfaces to ensure reliable sealing during the high-temperature vacuum process, allowing for long-term gasket maintenance without replacement. Zirconium trays are clamped between the sections, with a liquid redistributor on top and supporting the structured ceramic packing inside the column, and a wall-blocking ring on the bottom. Through-holes are machined around the tray, connecting to the thermometer protection tubes of the zirconium material inside the column, allowing for temperature measurement via the tray structure. The column sections have a hollow cylindrical structure, facilitating the installation of structured ceramic packing within the column. This optimizes the gas-liquid contact conditions for the vacuum alcoholysis reaction, reducing gas velocity and pressure.

[0072] Furthermore, an emergency storage tank can be installed below the alcoholysis tower. In the event of an accident such as a power outage, the reactants in the alcoholysis tower can be quickly and completely discharged into the emergency storage tank by gravity, preventing them from remaining in the tower and undergoing a cross-linking and solidification reaction.

[0073] During the reaction, because the molar volume of the gas is large and the density is low under vacuum, a high gas velocity can be used in the alcoholysis tower to quickly drive away hydrogen chloride, and the liquid reaction time can be extended by increasing the tower height without increasing the contact time between alcohol and hydrogen chloride.

[0074] During operation, the continuous tower-type alcoholysis system for high-boiling-point chlorosilanes described in this invention can control a suitable vacuum level to make the boiling point of the liquid phase fluid very close to the alcoholysis reaction temperature, making it difficult to dissolve alcohol and hydrogen chloride gas. This makes it difficult for trace iron impurities remaining in the liquid phase to catalyze the reaction of alcohol and hydrogen chloride, while the partial pressure of alcohol and hydrogen chloride in the gas phase is very low, resulting in a slow reaction. Therefore, the alcoholysis reaction operating temperature can be increased to 150℃-220℃, thereby meeting the operating conditions of the tower reaction process for fully reacting high-boiling-point chlorosilanes in the boiling point state to convert them into high-boiling-point alkoxysilanes in the boiling point state.

[0075] The reduced pressure vacuum high-temperature reaction conditions used in Example 1 exceed the structural capacity of ordinary enamel-lined towers and can be used to handle difficult reactions, such as the alcoholysis of high-boiling-point chlorosilanes with higher alcohols. It allows alcohol vapor and hydrogen chloride to flow rapidly to the top of the tower, accelerating the reaction process, forming a reasonable distribution of products at each reaction stage and tower temperature along the tower height, making full use of the tower's mass transfer function. The temperature of the liquid phase flowing down the tower gradually rises during the downward flow process, promoting a deep alcoholysis reaction, thereby ensuring the low-cost processing capability of high-boiling-point chlorosilanes.

[0076] Example 1 uses a magnetically driven liquid ring vacuum pump to achieve the required vacuum level, avoiding the unreliability of dynamic seals. Depending on the needs, different vacuum pumps can be used individually or in combination. Multiple units can be connected in parallel to share a single gas-liquid separator to meet high pumping capacity requirements, or they can be assembled into series to achieve even higher vacuum levels.

[0077] Furthermore, since the magnetic liquid ring vacuum pump requires the use of high-boiling-point raw material chlorosilane as the working liquid, this invention sets up a dechlorosilane tower. The tower selects saturated alkanes with low toxicity, which do not react with the raw material, can withstand high temperatures, and have very low freezing points. Through distillation and solvent action, it prevents the high-boiling-point chlorosilane with high melting point from solidifying and clogging when it reaches the low-temperature refrigeration condenser.

[0078] As some embodiments of the present invention, heptane can be selected as the saturated alkane used in the above-mentioned dechlorination silane tower. Heptane has low toxicity and a very low melting point. Hydrogen chloride has very low solubility in heptane. The boiling point of heptane is also not very high. It is easy to avoid reaching the bottom of the alcoholysis tower by the desorption of alcohol vapor.

[0079] Example 2

[0080] The equipment solution used in Example 1 above has a relatively high cost. For chlorosilanes with relatively low boiling and melting points, such as 1,2-(methyldichlorosilyl)ethane and 1,2-(trichlorosilyl)ethane, the reaction is easier when alcoholyzed with anhydrous methanol, and the product boiling point is not too high. In this case, a technical solution that reduces investment costs can be adopted, as detailed in [link to details]. Figure 2 Perform alcoholysis, specifically:

[0081] A continuous column-type alcoholysis system for high-boiling-point chlorosilanes, comprising:

[0082] The unit includes an alcohol pretreatment unit, a chlorosilane pretreatment unit, an alcoholysis unit, and an alcoholysis gas product treatment unit. The alcohol pretreatment unit is identical to that in Example 1 above, while the remaining units differ somewhat from those in Example 1. Specifically:

[0083] In the chlorosilane pretreatment unit, all chlorosilane raw materials from the chlorosilane raw material storage tank enter the falling film evaporator for pretreatment.

[0084] In the alcoholysis unit, the alcoholysis column includes an upper alcoholysis column and a lower alcoholysis column. The bottom of the upper alcoholysis column is connected to the upper part of the lower alcoholysis column via a pump 6. Alcohol vapor from the alcohol pretreatment unit is introduced into the lower part of the lower alcoholysis column, and chlorosilane from the chlorosilane pretreatment unit is introduced into the upper part of the upper alcoholysis column. During the alcoholysis reaction, the material at the bottom of the upper alcoholysis column is introduced into the lower alcoholysis column via pump 6 to continue the reaction, and the material from the top of the lower alcoholysis column is introduced into the lower part of the upper alcoholysis column to continue the reaction.

[0085] In addition, the bottom of the lower alcoholysis column is connected to the neutralization tank via pump 1. The liquid material discharged from the bottom of the lower alcoholysis column is further processed in the neutralization tank, and the alcoholysis gaseous product discharged from the top of the upper alcoholysis column enters the alcoholysis gaseous product processing unit for processing.

[0086] The alcoholysis gas product processing unit includes a dechlorinated silane lower column, a vacuum pump, a dechlorinated silane upper column, a membrane compressor, and a hydrogen chloride purification column. The alcoholysis gas product discharged from the upper part of the upper column is first fed into the upper part of a stripping column, then passes through the alcohol vaporizer and enters the dechlorinated silane lower column. After rectification in the lower column, the gas is pumped from the top of the lower column to the lower part of the upper column by the vacuum pump. The material discharged from the bottom of the lower column is fed into a falling film evaporator. After further rectification in the upper column, the resulting gas is discharged from the top of the upper column, enters the membrane compressor, is compressed by the membrane compressor, and then fed into the hydrogen chloride purification column for rectification. Additionally, the liquid material at the bottom of the upper column is fed into the upper part of the lower column.

[0087] As some embodiments of the present invention, the vacuum pump is a magnetically driven Roots vacuum pump.

[0088] Furthermore, the alcoholysis gas product processing unit also includes a saturated hydrocarbon feed tank, which stores saturated hydrocarbons. The saturated hydrocarbon feed tank is connected to the dechlorinated silane tower and is used to replenish a certain amount of saturated hydrocarbons into the dechlorinated silane tower when needed.

[0089] Furthermore, a refrigeration condenser is installed at the top of the hydrogen chloride purification tower, and a reboiler and a cooler are installed at the bottom. The material discharged from the membrane compressor is distilled through the hydrogen chloride purification tower, and the gas is discharged from the top of the hydrogen chloride purification tower into the refrigeration condenser. After being processed by the refrigeration condenser, it can be supplied as clean hydrogen chloride gas to hydrogen chloride users. The material discharged from the bottom of the hydrogen chloride purification tower enters the reboiler. After being heated by the reboiler, the gaseous material enters the hydrogen chloride purification tower, and the liquid material is discharged to the cooler for cooling.

[0090] Furthermore, the alcoholysis gas product processing unit further includes:

[0091] A chloroalkane tower, connected to the cooler, is used to distill the material discharged from the cooler.

[0092] Pump 7, which is disposed between the cooler and the chloroalkane tower, is used to pump the material in the cooler into the chloroalkane tower;

[0093] And a chloroalkane storage tank, which is connected to the top of the chloroalkane tower for collecting material discharged from the top of the chloroalkane tower.

[0094] Furthermore, the bottom of the chloroalkane tower is connected to the top of the dechlorinated silane upper tower, and the material discharged from the bottom of the chloroalkane tower is circulated into the top of the dechlorinated silane upper tower for processing.

[0095] As some embodiments of the present invention Figure 2 The alcoholysis process shown can be used as a methanol alcoholysis esterification process for high-boiling products that are byproducts of the addition-method vinylchlorosilane synthesis process.

[0096] Furthermore, in Example 2, a high-efficiency magnetic Roots vacuum pump with a large pumping capacity is selected to meet the low vacuum requirements, and an enamel-lined tower is used as the alcoholysis reactor. However, the tower tray structure clamped between the tower sections is similar to that in Example 1, still using zirconium metal trays. The cross-sectional design of the ring around the tray is H-shaped, meaning that the upper and lower sides of the ring have symmetrical U-shaped grooves. Flexible graphite gaskets with a thickness of more than 6 mm can be installed in the grooves. The upper and lower grooves are then assembled with the sealing surfaces of the upper and lower enamel-lined tower sections, respectively, so that the high-temperature resistant graphite gasket structure can maintain stability and ensure long-term use. In this example, the enamel-lined tower section adopts a simple hollow cylinder structure without connecting pipes, which reduces the manufacturing difficulty and facilitates the use of a corrosion-resistant layer that is difficult to sinter but has better high-temperature resistance, allowing the enamel-lined tower to be used at high temperatures for a long time.

[0097] Furthermore, the top and bottom sections of the enamel-lined tower, including the sections with connecting pipes, are made of zirconium, which minimizes stress on the enamel layer. Meanwhile, Figure 2 The alcoholysis system in the middle is designed with two tall single towers operating in series, which reduces the difficulty of equipment and pipeline layout and installation, and also makes the selection of pumps 5 and 6 easier.

[0098] Furthermore, the diaphragm compressor provided in Example 2 can be used to meet the needs of users with higher hydrogen chloride gas pressure heads, such as above 0.2 MPa, while the system and process flow in Example 1 can meet the needs of hydrogen chloride users with hydrogen chloride pressure head requirements below 0.2 MPa.

[0099] Example 3

[0100] Based on Examples 1 and 2, the present invention also provides a continuous column alcoholysis system and method combining Examples 1 and 2, specifically as follows: Figure 3 As shown:

[0101] A continuous column-type alcoholysis system for high-boiling-point chlorosilanes, comprising:

[0102] Alcohol pretreatment unit, chlorosilane pretreatment unit, alcoholysis unit, and alcoholysis gas product processing unit.

[0103] The alcohol pretreatment unit is the same as in Example 1 above, while the other units differ from those in Example 1 above in certain ways, specifically:

[0104] In the chlorosilane pretreatment unit, the chlorosilane raw material from the chlorosilane raw material storage tank is first fed into the bottom of the dechlorosilane tower by pump 4 for distillation. The liquid material discharged from the bottom of the dechlorosilane tower is fed into the falling film evaporator. After being heated and vaporized in the falling film evaporator, it is discharged into the settling separator. After impurities are removed by the settling separator, the steam is discharged into the washing tower. After being washed and purified by the washing tower, it is fed into the stripping tower to remove light components, and the pretreated chlorosilane is obtained.

[0105] As some embodiments of this application, the pump 4 is a magnetically driven liquid ring vacuum pump assembly.

[0106] In the alcoholysis unit, the alcoholysis tower includes a zirconium metal alcoholysis tower and an enamel-lined alcoholysis tower. The bottom of the enamel-lined alcoholysis tower is connected to the top of the zirconium metal alcoholysis tower via a pump 6. Alcohol vapor from the alcohol pretreatment unit is introduced into the bottom of the zirconium metal alcoholysis tower, and chlorosilane from the chlorosilane pretreatment unit is introduced into the top of the enamel-lined alcoholysis tower. During the alcoholysis reaction, the material at the bottom of the enamel-lined alcoholysis tower is introduced into the zirconium metal alcoholysis tower via pump 6 to continue the reaction, and the material from the top of the zirconium metal alcoholysis tower is introduced into the enamel-lined alcoholysis tower to continue the reaction.

[0107] In addition, the bottom of the zirconium alcoholysis tower is connected to the neutralization tank via pump 1. The liquid material discharged from the bottom of the zirconium alcoholysis tower is further processed in the neutralization tank, and the alcoholysis gaseous product discharged from the top of the enamel alcoholysis tower enters the alcoholysis gaseous product processing unit for processing.

[0108] Furthermore, the alcoholysis unit also includes:

[0109] A sodium alkoxide feeding tank, connected to the neutralization tank, is used to inject sodium alkoxide into the neutralization tank;

[0110] Pump 1, located between the alcoholysis tower and the neutralization tank, is used to pump the liquid material at the bottom of the zirconium alcoholysis tower into the neutralization tank for neutralization reaction with sodium alkoxide.

[0111] As some embodiments of this application, the zirconium alcoholysis tower is also connected to the falling film reboiler for returning a portion of the material discharged from the zirconium alcoholysis tower to the falling film reboiler, where it mixes with the alcohol vapor in the falling film reboiler and is then reintroduced into the lower part of the zirconium alcoholysis tower. In this way, alcohol vapor and substances such as chlorosilanes can undergo pre-reaction in the falling film reboiler before entering the zirconium alcoholysis tower, thereby increasing the degree of reaction.

[0112] As some embodiments of this application, the neutralization tank can be one or multiple tanks arranged in parallel, such as neutralization tank 1, neutralization tank 2 and neutralization tank 3 arranged in parallel.

[0113] As some embodiments of this application, the alcoholysis unit further includes: a crude esterification product storage tank, wherein the material in the neutralization tank is neutralized with sodium alkoxide and then discharged into the crude esterification product storage tank.

[0114] As some embodiments of this application, the alcoholysis unit further includes an emergency storage tank located below the alcoholysis tower. In the event of an accident such as a power outage, the reactants in the alcoholysis tower can be quickly and completely discharged into the emergency storage tank by gravity to prevent them from remaining in the tower and undergoing a cross-linking and solidification reaction.

[0115] Furthermore, in the alcoholysis gas product processing unit, the alcoholysis gas product discharged from the top of the enamel alcoholysis tower is first fed into the upper part of the stripping tower, and then pumped into the dechlorination silane tower by the pump 4. In the dechlorination silane tower, it is mixed with the material from the chlorosilane raw material storage tank and subjected to distillation. The liquid material discharged from the bottom of the dechlorination silane tower enters the falling film evaporator. The gaseous material discharged from the top of the dechlorination silane tower is sent into the stripping tower 2 by a magnetically driven Roots vacuum pump. Meanwhile, for easy distinction, the stripping tower located between the alcohol vaporizer and the iron-removed chlorosilane storage tank is referred to as stripping tower 1. After the gaseous material from the dechlorination silane tower is de-lightened in the stripping tower 2, the resulting gaseous material enters the refrigeration condenser 1 for processing, and then enters the membrane compressor. After being compressed by the membrane compressor, it enters the heater for heating treatment. The gaseous material in the heater enters the hydrogen chloride purification tower for distillation treatment, and the liquid material in the heater enters the chloroalkane separation system for distillation treatment. The liquid material produced by the stripping tower 2 is fed into the dechlorinated silane tower.

[0116] Specifically, the gaseous material produced by the hydrogen chloride purification tower is sent to the hydrogen chloride user after passing through the refrigeration condenser 2; the liquid material produced by the hydrogen chloride purification tower is discharged to the flash evaporator for further processing.

[0117] Furthermore, the gas discharged from the top of the flash tower is introduced into the upper part of the stripping tower 2; the liquid material at the bottom of the flash tower enters the alkane storage tank.

[0118] Furthermore, the alkane storage tank can feed the material inside into a dechlorination silane tower for its use.

[0119] Furthermore, the gaseous material produced by the distillation of the chloroalkane separation system is fed into a chloroalkane storage tank for storage; the liquid material produced by the distillation of the chloroalkane separation system is fed into an alkane storage tank.

[0120] Example 3 is particularly suitable for alcoholysis processes with slow reaction rates, high boiling points of materials, high reaction temperatures, and high vacuum requirements. It adopts a similar enamel-lined tower structure to Example 2. The initial alcoholysis reaction is first completed using an enamel-lined tower, and then a reaction tower with the zirconium metal tower body material from Example 1 or a high-temperature resistant impermeable graphite tower is used to carry out a high-temperature reaction to complete the deep alcoholysis reaction.

[0121] Furthermore, the vacuuming and gas compression system shown in Example 3 can be used to achieve high vacuum and high flow rate gas compression processes. In actual production, the methods of Example 1 and Example 2 can be simplified as needed to obtain a more reasonable configuration.

[0122] In addition to the basic piping configurations shown in the above embodiments and figures, the present invention also includes a small number of auxiliary devices and pipelines, as detailed in Embodiments 4 and 5 below. These auxiliary devices and pipelines are used to facilitate the start-up and shutdown of the device and to ensure the reliability of the device's long-term stable operation.

[0123] Example 4

[0124] like Figure 4 As shown, an auxiliary system for an alcohol vaporizer is presented, specifically:

[0125] Liquid alcohol from pump 3 is fed into the alcohol vaporizer and vaporized through heat exchange. After vaporization, it is discharged to the alcohol vapor demister for demisting, and then the resulting gaseous alcohol is fed into the alcohol superheater.

[0126] Simultaneously, gas from the top of the alcoholysis tower is introduced into the upper part of the stripping tower, and then enters the alcohol vaporizer for heat exchange. The non-condensable gas after passing through the vaporizer demagnetizes and drives the liquid ring vacuum pump. Liquid from the vaporizer enters a gas-liquid separator, and the liquid obtained after separation in the gas-liquid separator is again introduced into the vaporizer for heat exchange. A portion of the liquid obtained after separation in the gas-liquid separator is pumped into a candle filter, and the clean liquid after filtration is introduced into the vaporizer. Waste residue after filtration in the candle filter is discharged to a slag discharge tank. Another portion of the liquid obtained after separation in the gas-liquid separator is pumped into a jet booster as an ejector fluid to eject the remaining liquid from the gas-liquid separator. The material discharged from the jet booster enters an auxiliary water cooler for cooling, and then is discharged into the vaporizer.

[0127] Example 5

[0128] like Figure 5 As shown, an auxiliary system for a falling film evaporator is presented, specifically:

[0129] The mixed liquid from the bottom of the dechlorination silane tower, the mixed liquid from the bottom of the washing tower, and the chlorosilane liquid from pump 4 enter from the top of the falling film evaporator. After passing through the liquid distributor located at the top of the falling film evaporator, it is evenly sprayed into the falling film evaporator. After heat exchange in the heat exchange section of the falling film evaporator, it enters the gas-liquid separation zone at the bottom of the falling film evaporator. The gas generated in the gas-liquid separation zone goes to the bottom of the washing tower, and the liquid is pumped to the candle filter by a fluid pump. The clean liquid after being filtered by the candle filter is fed into the falling film evaporator, and the waste residue after being filtered by the candle filter is discharged to the slag discharge tank.

[0130] As some embodiments of the present invention, during startup, the following basic functions are achieved through an auxiliary system: first, saturated hydrocarbons are used in the washing tower and falling film evaporator system under normal pressure to clean the washing tower and stripping tower with saturated hydrocarbons, and clean saturated hydrocarbons are accumulated in the iron-removed chlorosilane storage tank. Then, this clean saturated hydrocarbons are used to enter the alcoholysis tower for reflux vaporization washing to clean the alcoholysis tower and at the same time increase the equipment temperature to create conditions for chlorosilane feeding.

[0131] In addition, the wastewater obtained from washing can be sent to a sedimentation separator for treatment. Then, the vacuum system is started to draw a vacuum, and chlorosilane is fed in and mixed with saturated hydrocarbons for reflux vaporization, so that the equipment temperature gradually rises to the reaction temperature. After the equipment is purified and the temperature and vacuum meet the reaction conditions, the feedstock alcohol is started, and the designed operating parameters are quickly adjusted to prevent the generated hydrogen chloride from contacting the alcohol for too long and causing side reactions.

[0132] This startup method avoids thermal shock to enamel-lined equipment, and significantly reduces the need for heat tracing and insulation on pipe and equipment surfaces when handling high-freezing-point chlorosilanes. This heat tracing and insulation is typically high-temperature resistant electric heating tape, used to ensure that the equipment can be preheated to meet startup requirements under varying temperature conditions.

[0133] The auxiliary water cooler in Embodiment 4 above can ensure the operational flexibility of the device and facilitate the start-up operation of the device. Figure 4 Figure 5 Candle filters can be used to maintain liquid cleanliness and prevent scale buildup on heat exchange tubes. In comparison, Figure 5 The improved equipment process method has significantly better reliability than... Figure 1 , Figure 2 and Figure 3 The process flow is shown.

[0134] In summary, the invention utilizes a zirconium metal alcoholysis tower to achieve the simplest single-tower liquid-phase delayed alcoholysis reaction system. By pre-removing iron, copper, and fluoride ion impurities from the raw materials through vaporization, demisting, or washing and distillation purification, zirconium metal exhibits strong corrosion resistance not only to hydrochloric acid of varying concentrations but also to alkalis at high temperatures. It can withstand thermal shock from drastic temperature changes, allowing for rapid adjustment of reactor feed parameters to quickly reach a stable and optimal operating state. This results in high reliability of the high-temperature, high-vacuum, and highly corrosive high-boiling-point chlorosilane alcoholysis reaction unit, strong adaptability to raw materials, and simplified operation and maintenance. Because it avoids the severe corrosion damage to on-site equipment caused by frequent maintenance and disassembly of highly corrosive chlorosilanes, it can serve as a highly reliable public system for rotating the alcoholysis and esterification of different chlorosilane materials, significantly reducing investment. It can not only process high-boiling-point chlorosilanes from a single plant but also provide services to other plants.

[0135] Secondly, the matching of zirconium trays, enamel sections, and high-temperature resistant flexible graphite pads in the alcoholysis tower structure can increase the single tower height of the enamel tower, enhance its applicability, ensure high-temperature operation reliability, and significantly reduce investment.

[0136] Third, the saturated hydrocarbon circulation system used in this invention eliminates the solidification and blockage of chlorosilanes, which is highly reliable and adaptable to raw materials. It can avoid the risk of thermal shock damage to enamel equipment, thereby significantly reducing equipment investment by using low-cost enamel structural components. It also reduces the difficulty of operation and is very beneficial for energy-saving design.

[0137] Fourth, this invention uses enamel towers, zirconium metal towers, and impermeable graphite towers in series to improve reliability and reduce the construction, operation, and maintenance costs of the equipment.

[0138] Fifth, the process flow design of this invention provides an economical and energy-saving special vacuum suction process suitable for the alcoholysis reaction of high-boiling-point and high-freezing-point chlorosilanes.

[0139] Sixth, the continuous alcoholysis reaction system for chlorosilanes provided by this invention has strong adaptability to processing different high-boiling-point chlorosilanes and low cost.

[0140] While the present invention has been disclosed above, it is not limited thereto. In the description of this specification, references to terms such as "one embodiment," "some embodiments," "illustrative embodiment," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Any person skilled in the art can make various modifications and alterations without departing from the spirit and scope of the present invention; therefore, the scope of protection of the present invention should be determined by the scope defined in the claims.

Claims

1. A continuous tower-type alcoholysis system for high-boiling-point chlorosilanes, characterized in that, include: The alcohol pretreatment unit includes an alcohol vaporizer, a demister, an alcohol superheater, and a falling film reboiler connected in sequence. After the alcohol raw material is vaporized by the alcohol vaporizer, it is passed into the demister for demisting treatment, and then passed into the alcohol superheater and the falling film reboiler for heating treatment to obtain pretreated alcohol vapor. The chlorosilane pretreatment unit includes a falling film evaporator, a settling separator, a washing tower, and a stripping tower. The chlorosilane raw material is first fed into the falling film evaporator and heated to vaporize. The unvaporized liquid is discharged into the settling separator. After impurities are removed by the settling separator, the steam is discharged into the washing tower. After washing and purification in the washing tower, it is fed into the stripping tower to remove light components, thus obtaining the pretreated chlorosilane. The alcoholysis unit includes an alcoholysis tower, a neutralization tank, and a crude esterification product storage tank connected in sequence. Pretreated alcohol vapor is introduced from the bottom of the alcoholysis tower, and pretreated chlorosilane liquid is introduced from the top of the alcoholysis tower. After the two undergo alcoholysis reaction in the alcoholysis tower, the resulting liquid material is discharged from the bottom of the alcoholysis tower into the neutralization tank. After neutralization with sodium alkoxide in the neutralization tank, it is discharged into the crude esterification product storage tank. Part of the chlorosilane purified by the settling separator is returned to the falling film evaporator; The remaining chlorosilane vapor is fed into the scrubbing tower for washing and purification treatment; The clean chlorosilane discharged from the top of the washing tower is fed into the stripping tower for further processing, and the material discharged from the bottom of the washing tower is returned to the falling film evaporator and enters the falling film evaporator together with the material from the chlorosilane raw material storage tank for processing. A pre-removed iron chlorosilane storage tank is provided at the bottom of the stripping tower, which stores the pre-removed iron chlorosilane. A portion of the material in the pre-removed iron chlorosilane storage tank is sent to the top of the alcoholysis tower for alcoholysis reaction, and another portion of the material is sent to the top of the washing tower to wash the gaseous material inside. The continuous tower alcoholysis system for high-boiling-point chlorosilanes also includes: The alcoholysis gas product processing unit includes a vacuum pump, a dechlorinated silane tower, and a hydrogen chloride purification tower. The alcoholysis gas product discharged from the top of the alcoholysis tower is first introduced into the top of the stripping tower, and then drawn into the dechlorinated silane tower by the vacuum pump. After being processed by the dechlorinated silane tower, it is discharged into the hydrogen chloride purification tower.

2. The continuous tower-type alcoholysis system for high-boiling-point chlorosilanes according to claim 1, characterized in that, Part of the material from the chlorosilane storage tank enters the falling film evaporator, while the other part enters the vacuum pump. After mixing with the alcoholysis gas products from the stripping tower, the mixture is discharged into the lower part of the dechlorinated silane tower via the vacuum pump. After being distilled in the dechlorinated silane tower, the gas is discharged from the upper part of the dechlorinated silane tower into the hydrogen chloride purification tower; the liquid is discharged from the lower part of the dechlorinated silane tower into the falling film evaporator.

3. The continuous tower alcoholysis system for high-boiling-point chlorosilanes according to claim 1, characterized in that, The alcoholysis column includes an upper alcoholysis column and a lower alcoholysis column. The bottom of the upper alcoholysis column is connected to the upper part of the lower alcoholysis column. Alcohol vapor from the alcohol pretreatment unit is introduced into the lower part of the lower alcoholysis column, and chlorosilane from the chlorosilane pretreatment unit is introduced into the upper part of the upper alcoholysis column. During the alcoholysis reaction, the material at the bottom of the upper alcoholysis column is introduced into the lower alcoholysis column to continue the reaction, and the material at the top of the lower alcoholysis column is introduced into the lower part of the upper alcoholysis column to continue the reaction. The bottom of the lower alcoholysis column is connected to the neutralization tank. The liquid material discharged from the bottom of the lower alcoholysis column is further processed in the neutralization tank, and the alcoholysis gaseous product discharged from the top of the upper alcoholysis column enters the alcoholysis gaseous product processing unit for processing.

4. The continuous tower-type alcoholysis system for high-boiling-point chlorosilanes according to claim 1 or 3, characterized in that, The alcoholysis gas product processing unit includes: a dechlorinated silane lower column, a vacuum pump, a dechlorinated silane upper column, a membrane compressor, and a hydrogen chloride purification column. The alcoholysis gas product discharged from the upper part of the alcoholysis column is first introduced into the upper part of the stripping column, then passes through the alcohol vaporizer and enters the dechlorinated silane lower column. After rectification in the dechlorinated silane lower column, the gas is pumped from the top of the dechlorinated silane lower column to the lower part of the dechlorinated silane upper column by the vacuum pump. The material discharged from the bottom of the dechlorinated silane lower column is introduced into the falling film evaporator. After the material is rectified again in the dechlorinated silane upper column, the resulting gas is discharged from the top of the dechlorinated silane upper column and enters the membrane compressor. After being compressed by the membrane compressor, it is introduced into the hydrogen chloride purification column for rectification. The liquid material at the bottom of the dechlorinated silane upper column is introduced into the upper part of the dechlorinated silane lower column.

5. The continuous tower-type alcoholysis system for high-boiling-point chlorosilanes according to claim 1, characterized in that, The alcoholysis tower includes a zirconium metal alcoholysis tower and an enamel-lined alcoholysis tower. The bottom of the enamel-lined alcoholysis tower is connected to the top of the zirconium metal alcoholysis tower. Alcohol vapor from the alcohol pretreatment unit is introduced into the bottom of the zirconium metal alcoholysis tower, and chlorosilane from the chlorosilane pretreatment unit is introduced into the top of the enamel-lined alcoholysis tower. During the alcoholysis reaction, the material at the bottom of the enamel-lined alcoholysis tower is introduced into the zirconium metal alcoholysis tower for further reaction, and the material at the top of the zirconium metal alcoholysis tower is introduced into the enamel-lined alcoholysis tower for further reaction. The bottom of the zirconium metal alcoholysis tower is connected to the neutralization tank. The liquid material discharged from the bottom of the zirconium metal alcoholysis tower is further processed in the neutralization tank, and the alcoholysis gaseous product discharged from the top of the enamel-lined alcoholysis tower enters the alcoholysis gaseous product processing unit for processing.

6. The continuous tower-type alcoholysis system for high-boiling-point chlorosilanes according to claim 1, characterized in that, The alcohol vaporizer, falling film reboiler, and stripping tower are made of zirconium, while the demister, alcohol superheater, and scrubbing tower are made of pure nickel.

7. A continuous column-type alcoholysis method for high-boiling-point chlorosilanes, characterized in that, The method employs the continuous tower alcoholysis system described in any one of claims 1 to 6 to perform alcoholysis of chlorosilanes.

Citation Information

Patent Citations

  • Alcoholysis process and device of chlorosilane

    CN116396322A