CN214004065U - Device for preparing high-purity germanium tetrachloride through disproportionation of trichlorogermane - Google Patents
Device for preparing high-purity germanium tetrachloride through disproportionation of trichlorogermane Download PDFInfo
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Abstract
The utility model relates to a device for preparing high-purity germanium tetrachloride by disproportionation of trichlorogermane. The device comprises a disproportionation reactor R101, a reaction condenser E101, a light component removal tower T201 and a refining tower T301 which are connected in sequence, wherein condensers are arranged on the tops of the light component removal tower T201 and the refining tower T301, and reboilers are arranged in a tower kettle. The high-purity germanium tetrachloride is prepared by adopting the disproportionation reaction of the trichlorogermane, so that the introduction of sulfuric acid and hydrochloric acid is avoided, three wastes are not generated, and the green degree of the production process is improved; through ultraviolet light catalytic reaction and chlorine gas introduction, the conversion rate of the trichlorogermane and the yield of the germanium tetrachloride are improved; hydrogen-containing impurities and metal impurities can be effectively removed at one time, and 5N-8N optical fiber-grade germanium tetrachloride is obtained through refining; the problem of high energy consumption caused by repeated distillation in the traditional process is avoided, and meanwhile, the green degree in the production process is improved.
Description
Technical Field
The utility model relates to a high-purity germanium tetrachloride preparation facilities, concretely relates to high-purity germanium tetrachloride's of disproportionation preparation of trichlorogermane device.
Background
Germanium tetrachloride (GeCl)4) Is one kind withoutThe color fuming liquid is commonly used as a dopant in the production of high-purity germanium dioxide, high-purity germanium and quartz optical fibers. With the development of modern communication industry, germanium tetrachloride as an optical fiber dopant has the advantages of large transmission capacity, high refractive index, low dispersion, low loss, strong anti-interference capability on nuclear radiation and electromagnetic radiation, all-weather working capability and the like, greatly improves the performance and quality of optical fibers, and rapidly increases the consumption of germanium in the field of optical fiber manufacturing. I.e. without high quality germanium tetrachloride, there is no high quality silica fiber. The non-ferrous metal trade mark (YS/T13-2007) divides the high-purity germanium tetrachloride into the following components according to the product purity and the proportion of metal-containing impurities: GeCl4-08 (impurity content is less than or equal to 2.0ng/g, purity is more than or equal to 99.999999 percent), GeCl4-07 (impurity content is less than or equal to 10 ng/g; purity is more than or equal to 99.99999%), GeCl4-05 (impurity content is less than or equal to 500ng/g, purity is more than or equal to 99.999%).
Chinese patent CN200810058153.6 proposes a method for producing germanium tetrachloride for optical fiber, which comprises the following steps: adding hydrochloric acid and germanium tetrachloride in a volume ratio of 0.25-2.0:1 into a distillation still for distillation, or introducing HCl gas while independently distilling the germanium tetrachloride until the distillation is finished, wherein the distillation temperature is 76-80 ℃, the distilled solution is stored in a storage tank after being separated by a hydrochloric acid separator, the solution needs to stand for 36-72 h and is discharged into an empty column distillation still, the temperature of the germanium tetrachloride solution is increased to 70-75 ℃, the illumination is carried out by an ultraviolet lamp while continuously introducing nitrogen for 12-36 h, and finally the product is rectified at 76-80 ℃ and is removed.
Chinese patent CN201210466977.3 proposes a system for producing optical fiber germanium tetrachloride, which greatly improves the rectification purity of optical fiber germanium tetrachloride by arranging a plurality of rectification units.
Chinese patent CN201611028826.4 proposes a process for preparing high-purity germanium tetrachloride by removing organic impurities and purifying, in which crude germanium tetrachloride produced by chlorination distillation of germanium concentrate is added into concentrated sulfuric acid for heating and primary distillation; adding analytically pure hydrochloric acid into the germanium tetrachloride produced by the primary distillation and introducing chlorine gas for primary re-distillation; repeating the step (2) to the germanium tetrachloride produced by the primary re-steaming for secondary re-steaming; adding concentrated sulfuric acid into germanium tetrachloride produced by secondary redistillation for secondary digestion and distillation; and (4) transferring germanium tetrachloride produced by secondary digestion and distillation, adding analytically pure concentrated sulfuric acid, and heating, rectifying and purifying. The method realizes the purpose of efficiently purifying the germanium tetrachloride to further remove organic impurities, and solves the problems that the product produced by the method for preparing the high-purity germanium tetrachloride by using the lignite containing germanium as the raw material and adopting the conventional production process is unqualified and the like.
The method adopts crude germanium tetrachloride produced by chlorination distillation of germanium concentrate as a raw material, and the germanium tetrachloride product is obtained by adding concentrated sulfuric acid and concentrated hydrochloric acid or introducing chlorine and hydrogen chloride for multiple times of distillation. The addition of concentrated sulfuric acid and concentrated hydrochloric acid has high requirements on equipment materials, the production cost is greatly increased, and a large amount of waste acid is generated to cause environmental pollution; repeated distillation for many times causes the problem of large energy consumption of the process.
To germanium tetrachloride's preparation problem, urgent need for utility model a device once only gets rid of contains hydrogen impurity and metallic impurity, reduces the requirement of synthesis, refining process to the equipment material, improves economic nature and production process's greenization degree, reduces the energy consumption simultaneously.
Disclosure of Invention
In order to solve the problems of the prior art, the utility model provides a device for preparing high-purity germanium tetrachloride by the disproportionation of trichlorogermane. The method comprises the steps of preparing germanium tetrachloride by taking trichlorogermane as a raw material through a disproportionation reaction, introducing chlorine to improve the conversion rate of the trichlorogermane and the yield of the germanium tetrachloride, and then removing light and refining to obtain a 5N-8N high-purity germanium tetrachloride product. The utility model avoids the introduction of sulfuric acid and hydrochloric acid, does not generate three wastes, and improves the green degree of the production process; and the hydrogen-containing impurities and metal impurities can be effectively removed at one time, so that the problem of high energy consumption caused by repeated distillation in the traditional process is solved.
In order to achieve the above object, the utility model adopts the following technical scheme to realize:
the utility model discloses a device of disproportionated preparation high-purity germanium tetrachloride of trichlorogermane, including the disproportionation reactor R101, reaction condenser E101, lightness-removing column T201, refined tower T301 that connect gradually, lightness-removing column T201 and refined tower T301 top of the tower all are provided with the condenser, and the tower cauldron all is provided with the reboiler.
The disproportionation reactor R101 is provided with a trichlorogermane inlet and an alcohol inlet, the lower part of the disproportionation reactor R101 is provided with a chlorine inlet, the top of the disproportionation reactor R is provided with a gas-phase material outlet, the bottom of the disproportionation reactor R is provided with a liquid-phase material outlet, the alcohol inlet is connected with the refining tower T301, the gas-phase material outlet is connected with the first condenser E101, and the liquid-phase material outlet is connected with the lightness-removing tower T201.
The first condenser E101 is provided with a material inlet and a material outlet, wherein the material inlet is connected with the disproportionation reactor R101, and the material outlet is connected with subsequent Cl2-an HCl recovery unit.
Lightness-removing tower T201 be equipped with the material import, the top is equipped with the top of the tower and adopts the export, upper portion is equipped with the backward flow mouth, the lower part is equipped with reboiler return opening, the bottom is equipped with the tower cauldron and adopts the export, wherein material access connection disproportionation reactor R101, the top of the tower is adopted the export, the backward flow mouth all is connected lightness-removing tower condenser E201, reboiler return opening is connected lightness-removing tower reboiler E202, the tower cauldron is adopted the export and is connected lightness-removing tower reboiler E202 all the way, connect refining tower T301 all the way.
Refining tower T301 be equipped with the material import, the top is equipped with the top of the tower and adopts the export, upper portion is equipped with the backward flow mouth, the lower part is equipped with reboiler return opening, the bottom is equipped with the cauldron and adopts the export, wherein material access connection takes off light tower T201, the top of the tower is adopted the export, the backward flow mouth all is connected refining tower condenser E301, refining tower reboiler E302 is connected to reboiler return opening, refining tower reboiler E302 is connected all the way to cauldron extraction opening, connect disproportionation reactor R101 all the way.
In the disproportionation reactor R101, the trichlorogermane is subjected to disproportionation reaction under the irradiation of ultraviolet light with the wavelength of 270nm-430nm and the catalysis of C4-C8 alcohol with the boiling point of more than 90 ℃ to generate germanium tetrachloride, germanium dichloride and hydrogen; filling chlorine into the disproportionation reaction unit during the disproportionation reaction, further reacting the chlorine with germanium dichloride generated by the disproportionation reaction to obtain germanium tetrachloride, and simultaneously reacting with hydrogen generated by the disproportionation reaction to obtain hydrogen chloride. The reaction pressure of the disproportionation reactor R101 is 0.15-0.5MPa, and the reaction temperature is 40-200 ℃.
The gas-phase product generated by the disproportionation reaction enters subsequent Cl2-HCl recovery, the liquid phase product of formation entering into the desorptionThe operating pressure of the light tower T201 and the light component removal tower T201 is 0.1-0.5 MPa, the temperature is 80-140 ℃, and the non-condensable gas extracted from the top of the light component removal tower T201 enters the subsequent Cl2And (3) recovering HCl, returning light components extracted from the tower top as raw materials to a disproportionation reactor R101, and feeding heavy components extracted from the tower bottom into a refining tower T301.
The operation pressure of the refining tower T301 is 0.1-0.3 MPa, and the temperature is 82-123 ℃. The high-purity germanium tetrachloride product with the purity of 5N-8N is extracted from the top of the refining tower T301, and the alcohols extracted from the bottom of the tower are returned to the disproportionation reactor R101.
A method for preparing high-purity germanium tetrachloride by disproportionation of trichlorogermane comprises the following steps:
(1) the trichlorogermane is subjected to disproportionation reaction under the irradiation of ultraviolet light and the catalysis of an alcohol medium to generate germanium tetrachloride, germanium dichloride and hydrogen; filling chlorine while carrying out disproportionation reaction, further reacting the chlorine with germanium dichloride generated by the disproportionation reaction to obtain germanium tetrachloride, and simultaneously reacting with hydrogen generated by the disproportionation reaction to obtain hydrogen chloride;
(2) performing light component removal treatment on a liquid-phase product generated by the disproportionation reaction, and returning a light component as a raw material for the disproportionation reaction; mixing the non-condensable gas with the gas phase product generated by the disproportionation reaction and recovering Cl2And HCl, the chlorine after recovery is used as the raw material of disproportionation reaction, and hydrogen chloride is used as the product to be extracted;
(3) refining the material after lightness removal under the conditions that the operating pressure is 0.1-0.3 MPa and the temperature is 82-123 ℃, extracting a high-purity germanium tetrachloride product with the purity of 5N-8N after refining, and simultaneously extracting alcohols to return to the disproportionation reaction.
The pressure of the disproportionation reaction is 0.15-0.5MPa, and the reaction temperature is 40-200 ℃.
The wavelength of the ultraviolet light is 270nm-430 nm.
The alcohol medium is C4-C8 alcohol with the boiling point of more than 90 ℃.
The mass ratio of the alcohols to the trichlorogermane is 0.5-3: 1.
The mol ratio of the chlorine to the trichlorogermane is 0.5-1: 1.
The light component removal treatment conditions are as follows: the operation pressure is 0.1-0.5 MPa, and the temperature is 80-140 ℃.
SaidRecovery of Cl2And the HCl conditions were: the operation pressure is 0.1-0.3 MPa, and the temperature is-80 to-50 ℃.
The utility model discloses a beneficial achievement is:
1. the high-purity germanium tetrachloride is prepared by adopting the disproportionation reaction of the trichlorogermane, the introduction of sulfuric acid and hydrochloric acid is avoided, three wastes are not generated, and the green degree of the production process is improved
2. Through ultraviolet light catalytic reaction and chlorine gas introduction, the conversion rate of the trichlorogermane and the yield of the germanium tetrachloride are improved.
3. Can effectively remove hydrogen-containing impurities and metal impurities at one time, and obtain 5N-8N optical fiber-grade germanium tetrachloride by refining.
4. The problem of high energy consumption caused by repeated distillation in the traditional process is avoided, and meanwhile, the green degree in the production process is improved.
Drawings
FIG. 1: a schematic diagram of a device for preparing high-purity germanium tetrachloride by disproportionation of trichlorogermane.
Detailed Description
As shown in fig. 1, the device for preparing high-purity germanium tetrachloride by disproportionation of trichlorogermane comprises a disproportionation reactor R101, a reaction condenser E101, a light component removal tower T201, a light component removal tower condenser E201, a light component removal tower reboiler E202, a refining tower T301, a refining tower condenser E301 and a refining tower reboiler E302.
The disproportionation reactor R101 is provided with a trichlorogermane inlet and an alcohol inlet, the lower part of the disproportionation reactor R101 is provided with a chlorine inlet, the top of the disproportionation reactor R is provided with a gas-phase material outlet, the bottom of the disproportionation reactor R is provided with a liquid-phase material outlet, the alcohol inlet is connected with the refining tower T301, the gas-phase material outlet is connected with the first condenser E101, and the liquid-phase material outlet is connected with the lightness-removing tower T.
The first condenser E101 is provided with a material inlet and a material outlet, wherein the material inlet is connected with the disproportionation reactor R101, and the material outlet is connected with subsequent Cl2-an HCl recovery unit.
Lightness-removing tower T201 be equipped with the material import, the top is equipped with the top of the tower and adopts the export, upper portion is equipped with the backward flow mouth, the lower part is equipped with reboiler return opening, the bottom is equipped with the tower cauldron and adopts the export, wherein material access connection disproportionation reactor R101, the top of the tower is adopted the export, the backward flow mouth all is connected lightness-removing tower condenser E201, reboiler return opening is connected lightness-removing tower reboiler E202, the tower cauldron is adopted the export and is connected lightness-removing tower reboiler E202 all the way, connect refining tower T301 all the way.
Refining tower T301 be equipped with the material import, the top is equipped with the top of the tower and adopts the export, upper portion is equipped with the backward flow mouth, the lower part is equipped with reboiler return opening, the bottom is equipped with the cauldron and adopts the export, wherein material access connection takes off light tower T201, the top of the tower is adopted the export, the backward flow mouth all is connected refining tower condenser E301, refining tower reboiler E302 is connected to reboiler return opening, refining tower reboiler E302 is connected all the way to cauldron extraction opening, connect disproportionation reactor R101 all the way.
The specific implementation mode is as follows:
(1) in a disproportionation reactor R101, the trichlorogermane is subjected to disproportionation reaction under the irradiation of ultraviolet light with the wavelength of 270nm-430nm and the catalysis of C4-C8 alcohol with the boiling point of more than 90 ℃ to generate germanium tetrachloride, germanium dichloride and hydrogen; filling chlorine into the disproportionation reaction unit during the disproportionation reaction, further reacting the chlorine with germanium dichloride generated by the disproportionation reaction to obtain germanium tetrachloride, and simultaneously reacting with hydrogen generated by the disproportionation reaction to obtain hydrogen chloride. The reaction pressure of the disproportionation reactor R101 is 0.15-0.5MPa, and the reaction temperature is 40-200 ℃.
The mass ratio of the disproportionation reaction unit alcohol to the trichlorogermane is 0.5-3: 1.
The molar ratio of chlorine to trichlorogermane in the disproportionation reaction unit is 0.5-1: 1.
(2) The gas-phase product generated by the disproportionation reaction enters subsequent Cl2Recovering HCl, feeding the generated liquid phase product into a light component removal tower T201, wherein the operating pressure of the light component removal tower T201 is 0.1-0.5 MPa, the temperature is 80-140 ℃, and non-condensable gas extracted from the top of the light component removal tower T201 enters subsequent Cl2And (3) recovering HCl, returning light components extracted from the tower top as raw materials to a disproportionation reactor R101, and feeding heavy components extracted from the tower bottom into a refining tower T301.
(3) The operation pressure of the refining tower T301 is 0.1-0.3 MPa, and the temperature is 82-123 ℃. The high-purity germanium tetrachloride product with the purity of 5N-8N is extracted from the top of the refining tower T301, and the alcohols extracted from the bottom of the tower are returned to the disproportionation reactor R101.
Example 1
The present invention will be further described with reference to fig. 1 and the following detailed description.
540g of trichlorogermane and 270g of n-butanol are added into a disproportionation reactor R101, 106.5g of chlorine gas is slowly introduced, the pressure of the disproportionation reactor R101 is controlled to be 0.15MPa, the temperature is controlled to be 40 ℃, and ultraviolet light with the wavelength of 270nm is used for irradiation. Gas-phase products (hydrogen chloride, chlorine, germanium tetrachloride and the like) generated by the reaction of the disproportionation reactor R101 enter Cl2An HCl recovery unit, wherein a liquid phase product generated by the reaction of the disproportionation reaction unit enters a lightness-removing tower T201, and the operating pressure and the temperature of the lightness-removing tower T201 are respectively 0.5MPa and 140 ℃. The noncondensable gas generated by the lightness-removing tower T201 enters Cl2An HCl recovery unit, wherein light components are used as raw materials and returned to a disproportionation reactor R101, and the materials after light removal enter a refining tower T301. The refining column T301 has an operating pressure of 0.3MPa and a temperature of 123 ℃. 450g of high-purity germanium tetrachloride product with the purity of 5N is extracted after the action of a refining tower T301, and simultaneously the extracted alcohols return to a disproportionation reactor R101.
Example 2
540g of trichlorogermane and 1620g of n-hexanol are added into a disproportionation reactor R101, 213g of chlorine gas is slowly introduced, the pressure of the disproportionation reactor R101 is controlled to be 0.5MPa, the temperature is controlled to be 200 ℃, and ultraviolet light with the wavelength of 330nm is used for irradiation. Gas-phase products (hydrogen chloride, chlorine, germanium tetrachloride and the like) generated by the reaction of the disproportionation reactor R101 enter Cl2HCl recovery Unit, Cl2-operating pressure of HCl recovery unit 0.2MPa, temperature-80 ℃. Liquid-phase products generated by the reaction of the disproportionation reactor R101 enter a lightness-removing tower T201, the operating pressure of the lightness-removing tower T201 is 0.1MPa, and the temperature is 80 ℃. The noncondensable gas generated by the lightness-removing tower T201 enters Cl2An HCl recovery unit, wherein light components are used as raw materials and returned to a disproportionation reactor R101, and the materials after light removal enter a refining tower T301. The operating pressure of the refining tower T301 is 0.1MPa, and the temperature is 82 ℃. 514.8g of high-purity germanium tetrachloride product with the purity of 8N is extracted after the action of a refining tower T301, and simultaneously, the extracted alcohols return to a disproportionation reactor R101.
Example 3
540g of trichlorogermane and 1620g of n-octanol are added into a disproportionation reactor R101, 180g of chlorine gas is slowly introduced, the pressure of the disproportionation reactor R101 is controlled to be 0.3MPa, the temperature is controlled to be 100 ℃, and ultraviolet light with the wavelength of 430nm is used for feedingAnd (4) line illumination. Gas-phase products (hydrogen chloride, chlorine, germanium tetrachloride and the like) generated by the reaction of the disproportionation reactor R101 enter Cl2HCl recovery Unit, Cl2-operating pressure of HCl recovery unit 0.3MPa, temperature-65 ℃. Liquid-phase products generated by the reaction of the disproportionation reactor R101 enter a lightness-removing tower T201, the operating pressure of the lightness-removing tower T201 is 0.3MPa, and the temperature is 123 ℃. The noncondensable gas generated by the lightness-removing tower T201 enters Cl2An HCl recovery unit, wherein light components are used as raw materials and returned to a disproportionation reactor R101, and the materials after light removal enter a refining tower T301. The refining column T301 was operated at 0.2MPa and 105 ℃. 482.6g of high-purity germanium tetrachloride with the purity of 7N is extracted after the action of a refining tower T301, and simultaneously the extracted alcohols return to a disproportionation reactor R101.
The technical solutions disclosed and proposed in the present invention can be implemented by those skilled in the art by referring to the contents of the text and appropriately changing the links such as condition and route, and although the method and preparation technique of the present invention have been described by the preferred embodiments, it is obvious for those skilled in the art to modify or recombine the method and technical route described herein without departing from the contents, spirit and scope of the present invention to realize the final preparation technique. 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 (5)
1. The device for preparing high-purity germanium tetrachloride through disproportionation of trichlorogermane is characterized by comprising a disproportionation reactor (R101), a reaction condenser (E101), a light component removal tower (T201) and a refining tower (T301) which are sequentially connected, wherein condensers are arranged on the tops of the light component removal tower (T201) and the refining tower (T301), and reboilers are arranged in tower kettles.
2. The apparatus as set forth in claim 1, wherein the disproportionation reactor (R101) is provided with a trichlorogermane inlet, an alcohol inlet, a chlorine inlet at the lower part, a gas phase material outlet at the top part, and a liquid phase material outlet at the bottom part, wherein the alcohol inlet is connected to the refining tower (T301), the gas phase material outlet is connected to the first condenser (E101), and the liquid phase material outlet is connected to the lightness-removing tower (T201).
3. The apparatus as claimed in claim 1, wherein the first condenser (E101) is provided with a material inlet and a material outlet, wherein the material inlet is connected to the disproportionation reactor (R101) and the material outlet is connected to the subsequent Cl2-an HCl recovery unit.
4. The apparatus as set forth in claim 1, wherein the lightness-removing column (T201) is provided with a material inlet, a top withdrawal outlet, a reflux outlet, a reboiler return outlet, and a bottom withdrawal outlet, wherein the material inlet is connected to the disproportionation reactor (R101), the top withdrawal outlet and the reflux outlet are connected to the lightness-removing column condenser (E201), the reboiler return outlet is connected to the lightness-removing column reboiler (E202), the bottom withdrawal outlet is connected to the lightness-removing column reboiler (E202) and the rectifying column (T301).
5. The apparatus as claimed in claim 1, wherein the refining tower (T301) is provided with a material inlet, a tower top outlet, a reflux inlet, a reboiler return inlet, and a tower bottom outlet, wherein the material inlet is connected with the lightness-removing tower (T201), the tower top outlet and the reflux inlet are both connected with the refining tower condenser (E301), the reboiler return inlet is connected with the refining tower reboiler (E302), the tower bottom outlet is connected with the refining tower reboiler (E302) in one way, and the disproportionation reactor (R101) in the other way.
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