CN210736200U - Device for preparing electronic grade hydrogen chloride by taking hydrogen chloride gas as raw material, which is byproduct of alcoholysis of organic chlorosilane - Google Patents
Device for preparing electronic grade hydrogen chloride by taking hydrogen chloride gas as raw material, which is byproduct of alcoholysis of organic chlorosilane Download PDFInfo
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Abstract
The utility model provides a device for preparing electronic-grade hydrogen chloride by taking hydrogen chloride gas as a by-product in alcoholysis of organic chlorosilane as a raw material. Comprises an absorption tower, a light component removal tower top condenser, a heavy component removal tower top condenser and a heat exchanger; taking hydrogen chloride gas as a byproduct of alcoholysis of organic chlorosilane as a raw material, adding the hydrogen chloride gas as the byproduct from the bottom of an absorption tower, and adding an absorbent from the top of the absorption tower; crude hydrogen chloride gas extracted from the tower top enters a light component removal tower; condensing the liquid phase material by a heat exchanger and a condenser to obtain reflux liquid at the top of the light component removal tower, extracting the gas phase material as light component impurities, extracting the light component removal tower kettle, and feeding the light component removal tower kettle into a heavy component removal tower; extracting the heavy component from the top of the heavy component removal tower and feeding the heavy component removal tower into a heavy component removal tower top condenser; after being condensed by a condenser, the liquid phase material flows back, and the gas phase hydrogen chloride is extracted as an electronic grade hydrogen chloride product. The device has simple process, is convenient for industrialized continuous operation, and improves the economic benefit and social benefit of enterprises.
Description
Technical Field
The utility model belongs to the electronic gas field relates to the preparation facilities of electron level hydrogen chloride, concretely relates to use the hydrogen chloride gas of organic chlorosilane alcoholysis byproduct to prepare the device of electron level hydrogen chloride as the raw materials.
Background
Organoalkoxysilane is one of the basic raw materials in the silicone industry, is an important raw material for synthesizing silane coupling agents, and can also be used for manufacturing silicone oil and polysilane to be used as optical fiber materials.
Alcoholysis of organochlorosilanes is one of the important means of preparing organoalkoxysilanes. The main reaction general formula is as follows:
RnSiCl4-n+(4-n)R′OH→RnSi(OR′)4-n+(4-n)HCl
wherein R is Me (methyl), Et (ethyl), Vi (vinyl), Pr (propyl), Bu (butyl), Ph (phenyl), Ac (acetyl), etc.; r' is Me, Et, Pr, PhOH and the like.
The organochlorosilane can produce hydrogen chloride as a byproduct in the alcoholysis process. The traditional alcoholysis process generally adopts an alkaline chemical reagent such as sodium hydroxide or sodium carbonate absorption neutralization process for treating the byproduct hydrogen chloride. The method has the advantages of high absorption speed, but can generate salt-containing waste water or solid waste which is difficult to treat, thereby not only increasing the cost, but also polluting the environment.
The patent CN201511031134.0 provides a method for purifying electronic grade hydrogen chloride, which comprises the steps of firstly introducing industrial grade hydrogen chloride with the purity of 99% into a first rectifying tower to remove light components, then enabling materials at the bottom of the first rectifying tower to enter a second rectifying tower to remove heavy components, collecting materials at the top of the second rectifying tower into an intermediate storage tank, and then removing other impurities from the materials in the intermediate storage tank through a plurality of molecular sieve adsorption towers to obtain a high-purity hydrogen chloride product with the purity of 99.9999%. The method has discontinuous integral process, and the process flow is complex and the energy consumption is higher when the method passes through a molecular sieve adsorption tower on the basis of rectification.
Patent CN02159980.7 proposes a method for preparing electronic grade hydrogen chloride, which uses petrochemical byproduct hydrogen chloride as raw material, in the presence of hydrogen chloride reaction catalyst, unsaturated hydrocarbon reacts with hydrogen chloride to convert into corresponding easy-to-remove halogenated hydrocarbon, and then the reaction product is separated and removed to obtain electronic grade hydrogen chloride with more than 5N. However, the method has low applicability, is only suitable for petrochemical industry by-product hydrogen chloride, comprises a separation process and a reaction process, and has complex process, high cost and high energy consumption.
Although the two methods can prepare the electronic-grade hydrogen chloride gas, both the methods have complex processes and technical defects, and are not suitable for preparing the electronic-grade hydrogen chloride by taking the hydrogen chloride gas as a byproduct in the alcoholysis of the organic chlorosilane as a raw material. Therefore, it is highly desirable to invent a method for preparing electronic grade hydrogen chloride by using hydrogen chloride gas generated by alcoholysis of organochlorosilane as a raw material.
Disclosure of Invention
An object of the utility model is to overcome prior art's not enough, provide a device that uses the hydrogen chloride gas of organic chlorosilane alcoholysis byproduct to prepare electron level hydrogen chloride as the raw materials preparation.
The utility model discloses a device for preparing electronic grade hydrogen chloride by taking hydrogen chloride gas of organic chlorosilane alcoholysis byproduct as raw material, including absorption tower T101, lightness-removing tower T102, T102 overhead condenser E201, weight-removing tower T103, T103 overhead condenser E301, heat exchanger E302, characterized by that absorption tower T101 upper portion is equipped with the absorbent import, and the lower part is equipped with byproduct hydrogen chloride import, and the top is equipped with the top of the tower export, and the bottom is equipped with the bottom of the tower cauldron and adopts the export, and wherein the bottom of the tower cauldron is adopted the export and is connected preceding device, and the top of the tower is adopted the export and is connected the middle part of lightness-removing; the middle part of the light component removal tower T102 is provided with a material inlet, the top part is provided with a tower top extraction outlet, the upper part is provided with a reflux port, the bottom part is provided with a tower kettle extraction outlet, the material inlet is connected with the top part of the absorption tower T101, the tower top extraction outlet is connected with the upper part of a heat exchanger E302, the reflux port is connected with a liquid phase outlet of a T102 tower top condenser E201, and the tower kettle extraction outlet is connected with the middle part of the heavy component removal tower; the condenser E201 at the top of the tower of the T102 is provided with a material inlet, a liquid phase outlet and a gas phase outlet, wherein the material inlet is connected with the lower part of the heat exchanger E302, the liquid phase outlet is connected with the upper part of the light component removal tower T102, and the gas phase outlet is used for extracting light impurities; the middle part of the heavy component removal tower T103 is provided with a material inlet, the top part is provided with a tower top extraction outlet, the upper part is provided with a reflux port, the lower part of the material is returned to the tower port, the bottom part is provided with a tower bottom extraction outlet, the material inlet is connected with the bottom part of the light component removal tower T102, the tower top extraction port is connected with a material inlet of a tower top condenser E301 of the T103, the reflux port is connected with a liquid phase material outlet of the tower top condenser E301 of the T103, the material is returned to the tower port and is connected with the top part of a heat exchanger E302, the tower; the T103 overhead condenser E301 is provided with a material inlet, a liquid phase outlet and a gas phase outlet, wherein the material inlet is connected with the top of the heavy component removal tower T103, the liquid phase outlet is connected with the upper part of the heavy component removal tower T103, and the gas phase outlet is used for producing an electronic grade hydrogen chloride product; the top of the heat exchanger E302 is provided with a cold material outlet, the upper part is provided with a hot material inlet, the lower part is provided with a hot material outlet, the bottom is provided with a cold material inlet, the cold material outlet is connected with the lower part of the heavy component removal tower T103, the hot material inlet is connected with the top of the light component removal tower T102, the hot material outlet is connected with the material inlet of a condenser E201 at the top of the T102 tower, and the cold material inlet is connected with the bottom of the heavy component removal tower T103.
The utility model discloses the technical scheme of the operation of device as follows:
(1) taking hydrogen chloride gas as a byproduct of alcoholysis of organic chlorosilane as a raw material, adding the hydrogen chloride gas as the byproduct from the bottom of an absorption tower T101, and adding an absorbent from the top of the absorption tower T101; crude hydrogen chloride gas extracted from the tower top enters a light component removal tower T102;
(2) the top of the lightness-removing tower T102 is taken as a heat source to enter a heat exchanger E302 to exchange heat with the bottom material of the weight-removing tower T103 and then enters a condenser E201 at the top of the T102, the liquid phase material is taken as the top reflux liquid of the lightness-removing tower T102 after the condensation of the heat exchanger E302 and the condenser E201, the gas phase material is taken as the light component impurity, and the bottom material of the weight-removing tower T102 is taken as the bottom reflux liquid of the weight-removing tower T103;
(3) the tower top of the heavy component removal tower T103 is extracted and enters a heavy component removal tower top condenser E301, and the heavy component removal tower top condenser is a partial condenser; after being condensed by a condenser, the liquid phase material flows back, and the gas phase hydrogen chloride is extracted as an electronic grade hydrogen chloride product.
The temperature of the top of the light component removing tower is higher than the temperature of the bottom of the heavy component removing tower by more than 10 ℃.
The mass ratio of the absorbent to the byproduct hydrogen chloride in the absorption tower is 1-10: 1.
The absorbent is alkoxy silane.
The tower top pressure of the absorption tower is 0.1-1 MPa.
The top pressure of the light component removal tower is 2-4 MPa.
The tower top pressure of the heavy component removing tower is 1-3 MPa.
The absorbent of the absorption tower T101 is from organoalkoxysilane generated by the preorder alcoholysis device.
According to the device for preparing the electronic-grade hydrogen chloride by using the hydrogen chloride gas as the byproduct of the alcoholysis of the organochlorosilane as the raw material, the absorbent is from the organoalkoxysilane in the preorder section, no external absorbent is needed to be added, the recovery rate of the byproduct hydrogen chloride gas is 90-99%, and the purity is more than or equal to 99.999%. Through the pressurized tower top gas phase heating atmospheric tower reboiler, not only can realize thermal reutilization, can save energy by more than 30%, practiced thrift the use of top of the tower low-temperature cooling medium simultaneously. The device has the advantages of simple and reliable process, no addition of external components, no waste water and solid generation, energy consumption reduction, cost saving, convenience for industrial continuous operation and improvement of economic benefits and social benefits of enterprises.
Drawings
FIG. 1: the schematic diagram of the device for preparing the electronic grade hydrogen chloride by using the hydrogen chloride gas which is the byproduct of the alcoholysis of the organic chlorosilane as the raw material.
The system comprises an absorption tower T101, a light component removal tower T102, a light component removal tower top condenser E201, a heavy component removal tower T103, a heavy component removal tower top condenser E301 and a heat exchanger E302.
Detailed Description
The present invention will be further described with reference to the following specific embodiments and with reference to fig. 1:
the device for preparing the electronic grade hydrogen chloride by taking the hydrogen chloride gas byproduct from the alcoholysis of the organic chlorosilane as the raw material comprises an absorption tower T101, a dehydrogenation tower T102, a tower top condenser E201 of the T102, a de-heavy tower T103, a tower top condenser E301 of the T103 and a heat exchanger E302. The upper part of the absorption tower T101 is provided with an absorbent inlet, the lower part is provided with a byproduct hydrogen chloride inlet, the top part is provided with a tower top extraction outlet, the bottom part is provided with a tower kettle extraction outlet, the tower kettle extraction outlet is connected with the preorder device, and the tower top extraction outlet is connected with the middle part of the lightness-removing tower T102; the middle part of the light component removal tower T102 is provided with a material inlet, the top part is provided with a tower top extraction outlet, the upper part is provided with a reflux port, the bottom part is provided with a tower kettle extraction outlet, the material inlet is connected with the top part of the absorption tower T101, the tower top extraction outlet is connected with the upper part of a heat exchanger E302, the reflux port is connected with a liquid phase outlet of a T102 tower top condenser E201, and the tower kettle extraction outlet is connected with the middle part of the heavy component removal tower; the condenser E201 at the top of the tower of the T102 is provided with a material inlet, a liquid phase outlet and a gas phase outlet, wherein the material inlet is connected with the lower part of the heat exchanger E302, the liquid phase outlet is connected with the upper part of the light component removal tower T102, and the gas phase outlet is used for extracting light impurities; the middle part of the heavy component removal tower T103 is provided with a material inlet, the top part is provided with a tower top extraction outlet, the upper part is provided with a reflux port, the lower part of the material is returned to the tower port, the bottom part is provided with a tower bottom extraction outlet, the material inlet is connected with the bottom part of the light component removal tower T102, the tower top extraction port is connected with a material inlet of a tower top condenser E301 of the T103, the reflux port is connected with a liquid phase material outlet of the tower top condenser E301 of the T103, the material is returned to the tower port and is connected with the top part of a heat exchanger E302, the tower; the T103 overhead condenser E301 is provided with a material inlet, a liquid phase outlet and a gas phase outlet, wherein the material inlet is connected with the top of the heavy component removal tower T103, the liquid phase outlet is connected with the upper part of the heavy component removal tower T103, and the gas phase outlet is used for producing an electronic grade hydrogen chloride product; the top of the heat exchanger E302 is provided with a cold material outlet, the upper part is provided with a hot material inlet, the lower part is provided with a hot material outlet, the bottom is provided with a cold material inlet, the cold material outlet is connected with the lower part of the heavy component removal tower T103, the hot material inlet is connected with the top of the light component removal tower T102, the hot material outlet is connected with the material inlet of a condenser E201 at the top of the T102 tower, and the cold material inlet is connected with the bottom of the heavy component removal tower T103.
The absorbent is organic alkoxy silane generated by a preorder alcoholysis device.
The mass ratio of the absorbent to the byproduct hydrogen chloride is 1-10: 1.
The tower top pressure of the absorption tower is 0.1-1 MPa;
the top pressure of the light component removal tower is 2-4 MPa;
the tower top pressure of the de-heavy tower is 1-3 MPa;
the temperature of the top of the light component removing tower is higher than the temperature of the bottom of the heavy component removing tower by more than 10 ℃.
According to the device for preparing the electronic-grade hydrogen chloride by taking the hydrogen chloride gas as the byproduct of the alcoholysis of the organochlorosilane as the raw material, the absorbent is from the organoalkoxysilane in the preorder section, no external absorbent is needed to be added, the recovery rate of the byproduct hydrogen chloride gas is 90-99%, the purity is more than or equal to 99.999%, and the energy consumption is reduced by more than 30% compared with that of the traditional process. The device has the advantages of simple and reliable process, no addition of external components, no waste water and solid generation, energy consumption reduction, cost saving, convenience for industrial continuous operation and improvement of economic benefits and social benefits of enterprises.
Example 1
(1) The byproduct hydrogen chloride is added from the bottom of the absorption tower T101, the absorbent is added from the top of the absorption tower T101, the tower top pressure of the absorption tower is 0.1MPa, the absorbent and the alcohol impurities extracted from the tower bottom return to the preceding alcoholysis device, and the crude hydrogen chloride gas extracted from the tower top enters the light component removal tower T102. (2) The pressure at the top of the light component removal tower T102 is 2MPa, the gas phase extracted at the top of the light component removal tower T102 is used as a heat source to enter a heat exchanger E302 to exchange heat with the material at the bottom of the heavy component removal tower T103 and then enter a condenser E201 at the top of the T102, the liquid phase is used as reflux liquid at the top of the light component removal tower T102 after condensation of the E302 and the E201, the gas phase is extracted as light component impurities, and the gas phase extracted at the bottom of the light component removal tower T102 enters the heavy component removal tower T103. (3) The pressure at the top of the heavy component removing tower T103 is 1MPa, the gas phase extracted from the top of the heavy component removing tower enters a heavy component removing tower top condenser E301, and the heavy component removing tower top condenser is a partial condenser. After condensation by a condenser, liquid phase reflows, and gas phase is taken as an electronic grade hydrogen chloride product and is extracted; heavy component impurities are extracted from the tower kettle of the de-heavy tower.
The mass ratio of the absorbing agent T101 in the absorption tower to the byproduct hydrogen chloride is 1:1
The top temperature of the light component removing tower is higher than the bottom temperature of the heavy component removing tower by 21 ℃.
The recovery rate of the byproduct hydrogen chloride gas reaches 90%, the purity is more than or equal to 99.999%, and the energy consumption is reduced by more than 30% compared with the traditional process.
Example 2
(1) The byproduct hydrogen chloride is added from the bottom of the absorption tower T101, the absorbent is added from the top of the absorption tower T101, the tower top pressure of the absorption tower is 0.5MPa, the absorbent and the alcohol impurities extracted from the tower bottom return to the preceding alcoholysis device, and the crude hydrogen chloride gas extracted from the tower top enters the light component removal tower T102. (2) The pressure at the top of the light component removal tower T102 is 4MPa, the gas phase extracted at the top of the light component removal tower T102 is used as a heat source to enter a heat exchanger E302 to exchange heat with the material at the bottom of the heavy component removal tower T103 and then enter a condenser E201 at the top of the T102, the liquid phase is used as reflux liquid at the top of the light component removal tower T102 after condensation of the E302 and the E201, the gas phase is extracted as light component impurities, and the gas phase extracted at the bottom of the light component removal tower T102 enters the heavy component removal tower T103. (3) The pressure at the top of the heavy component removing tower T103 is 3MPa, the gas phase extracted from the top of the heavy component removing tower enters a heavy component removing tower top condenser E301, and the heavy component removing tower top condenser is a partial condenser. After condensation by a condenser, liquid phase reflows, and gas phase is taken as an electronic grade hydrogen chloride product and is extracted; heavy component impurities are extracted from the tower kettle of the de-heavy tower.
The mass ratio of the absorbent T101 in the absorption tower to the byproduct hydrogen chloride is 5:1
The top temperature of the light component removing tower is 11 ℃ higher than the bottom temperature of the heavy component removing tower.
The recovery rate of the byproduct hydrogen chloride gas reaches 99%, the purity is more than or equal to 99.999%, and the energy consumption is reduced by more than 30% compared with the traditional process.
Example 3
(1) The byproduct hydrogen chloride is added from the bottom of the absorption tower T101, the absorbent is added from the top of the absorption tower T101, the tower top pressure of the absorption tower is 0.5MPa, the absorbent and the alcohol impurities extracted from the tower bottom return to the preceding alcoholysis device, and the crude hydrogen chloride gas extracted from the tower top enters the light component removal tower T102. (2) The pressure at the top of the light component removal tower T102 is 3MPa, the gas phase extracted at the top of the light component removal tower T102 enters a heat exchanger E302 as a heat source to exchange heat with the material at the bottom of the heavy component removal tower T103 and then enters a condenser E201 at the top of the T102, the liquid phase is used as reflux liquid at the top of the light component removal tower T102 after condensation of the E302 and the E201, the gas phase is extracted as light component impurities, and the gas phase extracted at the bottom of the light component removal tower T102 enters the heavy component removal tower T103. (3) The pressure at the top of the heavy component removing tower T103 is 2MPa, gas phase extracted from the top of the heavy component removing tower enters a heavy component removing tower top condenser E301, and the heavy component removing tower top condenser is a partial condenser. After condensation by a condenser, liquid phase reflows, and gas phase is taken as an electronic grade hydrogen chloride product and is extracted; heavy component impurities are extracted from the tower kettle of the de-heavy tower.
The mass ratio of the absorbent T101 in the absorption tower to the byproduct hydrogen chloride is 10:1
The top temperature of the light component removing tower is 14 ℃ higher than the bottom temperature of the heavy component removing tower.
The recovery rate of the byproduct hydrogen chloride gas reaches 95%, the purity is more than or equal to 99.999%, and the energy consumption is reduced by more than 30% compared with the traditional process.
According to the device for preparing the electronic-grade hydrogen chloride by using the hydrogen chloride gas as the byproduct of the alcoholysis of the organochlorosilane as the raw material, the absorbent is from the organoalkoxysilane in the preorder section, no external absorbent is needed to be added, the recovery rate of the byproduct hydrogen chloride gas is 90-99%, the purity is more than or equal to 99.999%, and the energy consumption is reduced by more than 30% compared with that of the traditional process. The device has the advantages of simple and reliable process, no addition of external components, no waste water and solid generation, energy consumption reduction, cost saving, convenience for industrial continuous operation and improvement of economic benefits and social benefits of enterprises.
The present invention discloses and provides a device for preparing electronic grade hydrogen chloride by using hydrogen chloride gas as a byproduct of alcoholysis of organic chlorosilane as a raw material, wherein a person skilled in the art can appropriately change the conditions and routes for reference, although the method and the preparation technology of the present invention have been described by way of preferred embodiments, it is obvious that the related person can modify or recombine the method and the technical routes described herein without departing from the contents, spirit and scope of the present invention to realize the final preparation technology. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (1)
1. The device for preparing the electronic-grade hydrogen chloride by taking the hydrogen chloride gas as the byproduct of the alcoholysis of the organic chlorosilane as the raw material comprises an absorption tower (T101), a light component removal tower (T102), a light component removal tower top condenser (E201), a heavy component removal tower (T103), a heavy component removal tower top condenser (E301) and a heat exchanger (E302), and is characterized in that the upper part of the absorption tower (T101) is provided with an absorbent inlet, the lower part of the absorption tower (T101) is provided with a byproduct hydrogen chloride inlet, the top of the absorption tower is provided with a tower top extraction outlet, the bottom of the absorption tower is provided with a tower bottom extraction outlet, the tower bottom extraction outlet is connected with a preo; the middle part of the light component removal tower (T102) is provided with a material inlet, the top part is provided with a tower top extraction outlet, the upper part is provided with a reflux port, the bottom part is provided with a tower kettle extraction outlet, the material inlet is connected with the top part of the absorption tower (T101), the tower top extraction outlet is connected with the upper part of the heat exchanger (E302), the reflux port is connected with a liquid phase outlet of a condenser (E201) at the top part of the light component removal tower, and the tower kettle extraction outlet is connected with the middle part of the heavy component removal; the condenser (E201) at the top of the light component removal tower is provided with a material inlet, a liquid phase outlet and a gas phase outlet, wherein the material inlet is connected with the lower part of the heat exchanger (E302), the liquid phase outlet is connected with the upper part of the light component removal tower (T102), and the gas phase outlet is used for extracting light impurities; the middle part of the heavy component removal tower (T103) is provided with a material inlet, the top part is provided with a tower top extraction outlet, the upper part is provided with a reflux port, the lower part of the material returns to a tower port, the bottom part is provided with a tower kettle extraction outlet, the material inlet is connected with the bottom part of the light component removal tower (T102), the tower top extraction port is connected with a material inlet of a tower top condenser (E301) of the heavy component removal tower, the reflux port is connected with a liquid phase material outlet of the tower top condenser (E301) of the heavy component removal tower, the material returns to the tower port and is connected with the top part of the heat exchanger (E302), the tower kettle extraction outlet is; the condenser (E301) at the top of the heavy component removal tower is provided with a material inlet, a liquid phase outlet and a gas phase outlet, wherein the material inlet is connected with the top of the heavy component removal tower (T103), the liquid phase outlet is connected with the upper part of the heavy component removal tower (T103), and the gas phase outlet is used for extracting an electronic grade hydrogen chloride product; the top of the heat exchanger (E302) is provided with a cold material outlet, the upper part of the heat exchanger is provided with a hot material inlet, the lower part of the heat exchanger is provided with a hot material outlet, the bottom of the heat exchanger is provided with a cold material inlet, the cold material outlet is connected with the lower part of the heavy component removal tower (T103), the hot material inlet is connected with the top of the light component removal tower (T102), the hot material outlet is connected with the material inlet of a condenser (E201) at the top of the light component removal tower, and the cold material inlet is connected with the bottom of the.
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| CN201920809033.9U CN210736200U (en) | 2019-05-29 | 2019-05-29 | Device for preparing electronic grade hydrogen chloride by taking hydrogen chloride gas as raw material, which is byproduct of alcoholysis of organic chlorosilane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110078024A (en) * | 2019-05-29 | 2019-08-02 | 天津中科拓新科技有限公司 | The method and device of electronic grade hydrogen chloride is prepared using the hydrogen chloride gas of organochlorosilane alcoholysis by-product as raw material |
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| CN110078024A (en) * | 2019-05-29 | 2019-08-02 | 天津中科拓新科技有限公司 | The method and device of electronic grade hydrogen chloride is prepared using the hydrogen chloride gas of organochlorosilane alcoholysis by-product as raw material |
| CN110078024B (en) * | 2019-05-29 | 2024-05-07 | 天津中科拓新科技有限公司 | Method and device for preparing electronic grade hydrogen chloride by taking hydrogen chloride gas as byproduct of organochlorosilane alcoholysis as raw material |
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