CN1511780A - Process for preparing electronic grade hydrogen chloride - Google Patents
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- CN1511780A CN1511780A CNA021599807A CN02159980A CN1511780A CN 1511780 A CN1511780 A CN 1511780A CN A021599807 A CNA021599807 A CN A021599807A CN 02159980 A CN02159980 A CN 02159980A CN 1511780 A CN1511780 A CN 1511780A
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Abstract
The preparation process of electronic grade hydrogen chloride with hydrogen chloride side product from petrochemical production as material includes the reaction of unsaturated hydrocarbon and hydrogen chloride to produce easy-to-eliminate hydrocarbon chloride in the condition of existing hydrogen chloride reaction catalyst and subsequent separation and elimination of reaction product. Before the reaction, the light and heavy components may be eliminated physically in advance. The said technological process can obtain 5N and over electronic grade hydrogen chloride product. Adding no reaction medium avoids the introduction of the other impurity, and the operation process is simple and low in cost.
Description
Technical Field
The invention relates to a method for preparing electronic grade hydrogen chloride, in particular to a method for preparing electronic grade hydrogen chloride by removing acetylene and ethylene impurities from petrochemical industry byproduct hydrogen chloride.
Background
High-purity hydrogen chloride is an important material for processes of silicon chip etching, passivation, epitaxy and the like in integrated circuit production, and can also be used in the fields of metal smelting, photoconductive communication, scientific research and the like. With the development of large-scale integrated circuits, the requirement on the purity of hydrogen chloride is higher and higher, the requirement on the content of impurities in the hydrogen chloride is more and more strict, and the requirements on the strict limitation of hydrocarbon (THC) and carbon oxidation are particularly requiredCompound (CO)X) To prevent C formation during wafer processing. Table 1 lists the standards of implementation of 5N electronic grade hydrogen chloride in the domestic market at present.
TABLE 1 Chinese market 5N electronic grade Hydrogen chloride respective company execution Standard
| Company(s) | Purity of ％ | Impurity ppm | ||||||
| N2 | O2Or (O2+Ar) | H2O | CO | CO2 | CH4Or (THC) | H2 | ||
| The gas industry of Beijing Hepu Beibei province has Limited company (executive American APCI standard) Quasi), AIR PRODUCTS | ≥ 99.999 | ＜2.0 | (＜1.0) | ＜1.0 | ＜1.0 | ＜2.0 | ＜1.0 | - |
| The Beijing Prexix practical gas is Limited company (Perform PRAXAIR USA) Standard), praxaair | ≥ 99.999 | ＜2.0 | ＜1.0 | ＜1.0 | ＜2.0 | ＜2.0 | ＜1.0 | - |
| Matheson Electronic, USA Products Group | ≥ 99.999 | ＜1.5 | (＜1.0) | ＜1.0 | ＜1.0 | ＜2.0 | ＜0.1 | - |
| French liquefied air Chinese Limited bus AIR liquid | ≥ 99.999 | ＜0.5 | ＜0.5 | ＜1.0 | - | ＜1.0 | (＜0.1) | ＜1.0 |
| Soltronic Chemikalien die Elektronic GmbH | ≥ 99.999 | ＜4.0 | (＜1.0) | ＜1.0 | - | ＜5.0 | (＜1.0) | - |
As can be seen from Table 1, (1) 5N electronic grade hydrogen chloride sold in domestic markets is from the United states, France or Germany, needs long-distance transportation and is expensive; (2) all products contained more CO2And (or) CO.
At present, two main raw materials are used for preparing high-purity hydrogen chloride. One is conventionally made of Cl2And H2The synthesized hydrogen chloride synthesis gas has high water content, serious corrosion, high requirement on equipment and high production cost. The other is byproduct hydrogen chloride gas of petrochemical industry, wherein the water content is low, the hydrogen chloride gas has no corrosion to stainless steel and carbon steel basically, but acetylene and ethylene impurities of 1000ppm or more are contained in the hydrogen chloride gas. The purification of the gas usually adopts a rectification or adsorption method, but because the boiling points of acetylene and ethylene impurities are close to the boiling point of hydrogen chloride, the acetylene and ethylene impurities are difficult to be removed cleanly by adopting the rectification method, and the adsorption method has the disadvantages of complicated operation process, frequent replacement of the adsorbent and high production cost.
US4065513 discloses a process for removing acetylene from hydrogen chloride gas. The patent adopts a process of chlorination reaction between added chlorine and acetylene and separation of reaction products to remove acetylene in the presence of activated carbon, so that the acetylene content can be reduced from 200-4000 ppm to below 50ppm, but the requirement of electron electrode hydrogen chloride is far less met. In addition, the method introducesan additive chlorine gas into the system, and increases the difficulty of purification.
US4839153 discloses a process for the purification of hydrogen chloride. In the method, acetylene is converted by hydrogenation, but the ethane is difficult to remove, and the product still contains ethane impurities of more than 2000ppm and cannot meet the requirement of electron electrode hydrogen chloride.
US patent 4986975 provides a process for the purification of hydrogen chloride obtained by pyrolysis of 1, 2-dichloroethane. In the method, the hydrogen chloride containing impurities reacts with extra excessive chlorine in the presence of a catalyst, the excessive chlorine reacts with olefin or chloroethylene, and finally rectification separation is carried out. The method needs additional chlorine in the first step of reaction and additional olefin or chloroethylene in the second step of reaction to convert the excessive chlorine. This not only requires the addition of a gaseous medium, but also adds a number of equipment loads and operating steps, increasing the cost of purification.
Disclosure of Invention
It is an object of the present invention to provide a process for the preparation of electronic grade hydrogen chloride. In particular to a method for preparing electronic grade hydrogen chloride by removing ethylene and acetylene from petrochemical industry byproduct hydrogen chloride. The ethylene and acetylene gas are removed without introducing other impurities, and the hydrogen chloride gas is purified.
Another object of the present invention is to provide an apparatus for producing electronic grade hydrogen chloride.
The process of the present invention comprises the conventional step of physically separating impurities from hydrogen chloride, such as adsorptive separation, distillation/rectification separation or a combination thereof, and is characterized by further comprising the step of reacting unsaturated hydrocarbons in the feed with hydrogen chloride in the presence of a hydrochlorination catalyst and subsequently removing the impurities. The unsaturated hydrocarbons include acetylene and ethylene, and the reaction with hydrogen chloride is carried out by: the method comprises the steps of firstly carrying out hydrochlorination of acetylene in the presence of a hydrochlorination catalyst to generate a reaction product which is easy to remove from hydrogen chloride, and then carrying out hydrochlorination of ethylene in the presence of a hydrochlorination catalyst to generate a reaction product which is easy to remove from hydrogen chloride. The reaction product is removed by distillation/rectification and/or adsorption.
The catalyst for hydrochlorination of acetylene should meet the requirement that the conversion rate of acetylene is not less than 95%, preferably not less than 99% under standard reaction conditions: an isothermal bed reactor with a diameter of 30X 300mm was used, 10g of catalyst was packed in the constant temperature section, and the remainder was packed with glass or ceramic balls. 1000ppm of acetylene was made up in 5N electronic grade hydrogen chloride as standard reactant. The reaction conditions were atmospheric pressure, 130 ℃ and a standard reactant flow rate of 15kg/h kgcat. Any conventional acetylene hydrochlorination catalyst satisfying the above conditions may be used, and for example, a catalyst in which a transition metal halide is supported on a porous carrier, preferably HgCl2-BaCl2Active carbon composite catalyst. BaCl is preferably controlled2/HgCl20.1-0.5/1 ═ active carbon2/10, preferably 0.2/1.25/10. The reaction conditions of the acetylene hydrochlorination reaction are as follows: the pressure P is 0.1-7.0 MPa, the temperature T is 130-180 ℃, and the space velocity W of the raw materials is less than or equal to 90 kg/h.kg cat.
The following reactions mainly take place over acetylene hydrochlorination catalysts:
when C in hydrogen chloride2H2At a content of less than 1000ppm, C2H2Can be fully transformed. In general, C at the outlet of the reactor2H2The content will be less than 1 ppm.
The catalyst used for the hydrochlorination of ethylene should meet the requirement of having an ethylene conversion of not less than 95%, preferably not less than 99%, under standard reaction conditions. The standard reaction conditions are as follows: an isothermal bed reactor with a diameter of 30X 300mm was used, 10g of catalyst was packed in the constant temperature section, and the remainder was packed with glass or ceramic balls. 100ppm of ethylene and about 50ppm of oxygen were made up in 5N electronic grade hydrogen chloride as standard reactant. The reaction conditions were atmospheric pressure, 210 ℃ and a standard reactant flow rate of 15 kg/h.kg cat. Any conventional ethylene hydrochlorination catalyst satisfying the above conditions may be used, and for example, a catalyst in which a transition metal halide is supported on a porous carrier, such as CuCl2-KCl-SrCl2An active carbon composite catalyst, wherein the atomic ratio of Sr/K/Cu is 0.1-1.0/0.1-2/1, preferably 0.5/1/1; CuCl2The weight ratio of the active carbon/the active carbon is 1 to 2.0/10, preferably 1.25 to 1.5/10. The operating conditions for the ethylene hydrochlorination were: the pressure is 0.1-7.0 MPa, the temperature T is 200-240 ℃, and the spacevelocity W of the raw material is less than or equal to 90 kg/h.kg cat. In addition, if the ethylene content in the feed is higher, a proper amount of O can be introduced into the deethylenizer2To contribute to the sufficiency of ethyleneAnd (4) reacting.
The following reactions mainly take place over ethylene hydrochlorination catalysts:
when a trace amount of oxygen is present in the hydrogen chloride,
when the hydrogen chloride is free of oxygen,
when C is contained in the hydrogen chloride2H4At a content of less than 10ppm, C2H4Sufficient conversion is achieved and, in general, the reactor outlet content can be below 1 ppm. For C2H4The hydrogen chloride gas with high content is properly mixed with O2In an amount of C2H4/O2＝1-2/1。
The reaction product is removed from the reaction mixture by conventional methods such as adsorption, distillation/rectification, etc. As the method of using the adsorption, any conventional adsorbent may be used, and the aforementioned acetylene and ethylene hydrochlorination catalyst may be used as the adsorbent. When the two catalysts are used as adsorbents, the operating conditions are that P is more than or equal to 0.5MPa, T is less than or equal to room temperature (the effect is better when the pressure is high and the temperature is low), the space velocity of raw materials is 0.06-0.1 kg/h.kg of the adsorbents, and the maximum adsorption capacity of the adsorbents on chlorinated hydrocarbons is 1.5kg/kg of the adsorbents.
In order to prolong the regeneration period of the adsorbent, the chlorinated hydrocarbon is preferably removed by rectification before the adsorption tank group so as to reduce the load of the adsorbent. The rectifying tower can adopt a common rectifying tower, and preferably adopts a regular packed tower with high plate efficiency.
In a preferred embodiment of the invention, the feed is preferably freed from light and heavy impurities other than ethylene and acetylene by physical separation, for example by distillation, before it is fed to the deethanizer and deethanizer reactor. The light component of interest is usually N2、O2、CH4Etc., heavy components such as CnHmClp、H2O, and the like.
According to another preferred embodiment of the present invention, the hydrogen chloride after the previous round of hydrochlorination and separation may be recycled as a feed to the next round of reaction-separation process in order to further improve the purity of the product. The scheme has the characteristics of strong adaptability to the actual purity, simplicity and feasibility, and can obtain electronic grade hydrogen chloride gas products with different purities according to the market demands.
In addition, the invention also provides equipment used in the electronic grade hydrogen chloride preparation method, which comprises a physical separation device and is characterized by comprising a hydrochlorination reaction device for carrying out hydrochlorination on unsaturated hydrocarbon contained in raw material hydrogen chloride with hydrogen chloride in the presence of a hydrochlorination catalyst, wherein an outlet of the hydrochlorination reaction device is connected with an inlet of the physical separation device. The hydrochlorination device is composed of an acetylene hydrochlorination reactor and an ethylene hydrochlorination reactor which are connected in sequence and connected with a physical separation device distillation/rectification and/or adsorption device behind the acetylene hydrochlorination reactor.
In one preferred embodiment, the hydrochlorination apparatus is preferably preceded by a device for removing light and heavy impurities from hydrogen chloride by physical separation, such as a light component removing distillation/rectification column and a heavy component removing distillation/rectification column.
In another preferred embodiment, a line is provided at the outlet of the physical separation device to connect to the inlet of the hydrochlorination reaction device to provide a passage for the hydrogen chloride from the previous reaction and separation to be fed to the next reaction.
The process method can obtain the electronic grade hydrogen chloride with the purity of more than 5N, has simple operation process, does not need additional reaction medium and has low production cost.
Drawings
FIG. 1 is a schematic flow chart of the production process of the present invention;
FIG. 2 is a schematic flow diagram of a preferred embodiment of the present invention.
Detailed Description
The invention is described in detail below with reference to specific examples, but it should be understood that the scope of the invention is not limited to the contents of the examples.
The raw materials, semi-finished products and finished product analysis method related to the patent adopt a method specified by national standard GB/T14602-93 of the people's republic of China.
EXAMPLE 1 removal of acetylene from Hydrogen chloride by hydrochlorination catalysis
A certain amount of acetylene was added to 5N electronic grade hydrogen chloride to form the raw material shown in Table 2
Table 2 starting material for example 1
| Name of impurity | N2 | O2 | H2O | CO | CO2 | CH4 | C2H2 |
| Content in ppm | 2.0 | 0.5 | 1.0 | 1.0 | 2.0 | 1.0 | 1000 |
Made by Beijing Huayu Tong chemical technology development Limited company under the name HY-01HgCl2-BaCl2The/active carbon composite catalyst is filled into a de-acetylene reactor to remove C in the de-acetylene reactor2H2. The reactor is an isothermal bed reactor with the size of phi 30 multiplied by 300mm, and 10g of catalyst is filled in a constant temperature section. The upper section of the reactor is provided with small ceramic balls with the diameter of 3mm, which is about 100mm and is used for gas distribution and raw material preheating. The lower section of the reactor is also provided with small ceramic balls with the diameter of 3mm and the diameter of 50 mm. The catalyst is filled in the middle constant temperature section. The reactor shell is heated by electric furnace wires, and the reaction temperature is strictly controlled. The reaction conditions were normal pressure, T130 deg.C, and the space velocity W of the feed gas 15 kg/h.kg cat. When the reaction gas at the outlet of the reactor is analyzed by the method specified in GB/T14602-93, C is not detected2H2While only 1.0ppm methane was detected.
Example 2 removal of ethylene from hydrogen chloride by hydrochlorination catalysis
A certain amount of ethylene and oxygen were added to 5N electronic grade hydrogen chloride to form the raw materials shown in Table 3.
Table 3 starting material for example 2
| Name of impurity | N2 | O2 | H2O | CO | CO2 | CH4 | C2H4 |
| Content in ppm | 2.0 | 50 | 1.0 | 1.0 | 2.0 | 1.0 | 100 |
The reactor used in example 1 was used, but a deethylenization catalyst of the type HY-02, manufactured by Beijing Kagaku Kogyo chemical engineering and technology development Co., Ltd, was charged therein. The reactor operating conditions were atmospheric pressure, T.210 ℃ and feed gas space velocity W.15 kg/h.kg cat. When the reaction gas at the outlet of the reactor is analyzed by the method specified in GB/T14602-93, C cannot be detected2H4While only about 1.0ppm methane was detected.
Example 3 removal of acetylene and ethylene from petrochemical by-product Hydrogen chloride
Referring to fig. 2, the petrochemical byproduct hydrogen chloride passes through a light component removal tower 1 and a heavy component removal tower 2, and after light components and heavy components are removed by rectification, the composition is shown in table 4.
Table 4 example 3 feedstock
| Name of impurity | N2 | O2 | H2O | CH4 | C2H2 | C2H4 |
| Content in ppm | 1.0 | 0.5 | 0.7 | 0.5 | 418.2 | 0.9 |
The feed gas has a particle size of 15m3The flow rate of/h (corresponding to 22 kg/h.kg cat) is sequentially removed with acetylene and ethylene by a de-acetylene reactor 3 and a de-ethylene reactor 4, and then cooled and buffered,the membrane compressor enters a dechlorination hydrocarbon tower 5 to remove reaction product halogenated hydrocarbon, the reaction product halogenated hydrocarbon is flashed by a flash tank 6, an adsorption tank group 7 is separated and passes through the membrane compressor, and finally the treated steel cylinder is filled.
The reactor 3 is a fixed bed reactor, 50kg of HY-01 catalyst is filled in the reactor, the effective height is 4500mm, the diameter is phi 195mm, the outer wall is heated by an electric furnace wire, phi 5mm and phi 3mm ceramic balls are filled in the upper section of 800mm, the catalyst is filled in the middle section, and phi 3mm ceramic balls are filled in the other lower sections. The operating pressure P is 0.75MPa and the temperature T is 160 ℃.
The reactor 4 and the reactor 3 are filled with 50kg of HY-02 catalyst, and the outer wall of the reactor is heated by an electric furnace wire. The operating pressure P was 0.7MPa and the temperature T was 235 ℃.
The dehalogenation hydrocarbon tower is a rectifying tower and is used for removing the chlorohydrocarbon generated by the reaction. The tower is filled with double-wire mesh regular packing, the height of the rectifying section is 3200mm, and the height of the stripping section is 800 mm. The tower kettle is heated by an electric furnace, and the tower top is cooled by water at 25 ℃. The operation pressure is 5.5MPa, the top temperature is 36 ℃, the kettle temperature is 38 ℃, the reflux amount is about 50kg/h, and the liquid phase at the top of the tower is extracted.
The adsorption tank group consists of 4 adsorption tanks connected in series and is used for removing the residual unsaturated hydrocarbon and chlorinated hydrocarbon. Each tank is 3000mm high and has a diameter of phi 195mm, and 50kg of HY-01 or HY-02 adsorbent is filled in the tank, and the total amount is 200 kg. The operating pressure is 0.5MPa and the temperature is room temperature.
The gas discharged by the adsorption tank group is compressed, cooled and liquefied by a membrane compressor, and then filled in a treated steel cylinder, so that the 5N electronic grade hydrogen chloride product is prepared.
The hydrogen chloride in the steel cylinder was analyzed by the method specified in GB/T14602-93, and the composition thereof is shown in Table 5.
Table 5 example 3 product composition
| Name of impurity | N2 | O2 | H2O | THC(CH4+C2H2) | COX |
| Content in ppm | 1.0 | - | 0.5 | 0.8 | - |
In the table, THC is mainly CH4And C is2H2The content of (A) is very small.
Example 4
The feed and the apparatus of example 3 were used, wherein the flow rate of the feed gas was 45m3At/h (corresponding to 66 kg/h.kg cat), the pressure in reactor 3 and reactor 4 was increased to 3.05MPa and 3.0MPa, respectively, and the temperature was varied by 140 ℃ and 210 ℃ respectively. THC in the product is 0.95ppm, wherein C2H2＝0.15ppm。
Example 5
Same as example 3, wherein the flow rate of the raw material gas was increased to 60m3At/h (corresponding to 88 kg/h. kg cat), the pressure in reactor 3 and reactor 4 was increased to 6.05MPa and 6.0MPa, respectively, and the temperature was changed to 150 ℃ and 220 ℃ respectively. The product only contains CH without passing through the adsorption tank group40.7ppm, but does not contain C2H2And C2H4。
Example 6
The product hydrogen chloride obtained in example 3 is used as a raw material and returned to the de-acetylene tower for circulation once. The operating conditions were the same as in example 3. The THC content in the obtained product is 0.6ppm, and C can not be detected2H2。
Example 7
The operation process is the same as that of example 3, wherein the product in the reactor is directly fed into the adsorption tank group without being fed into the dehydrohalogenation tower, and the operation pressure is 0.7MPa, so that the same product as that of example 3 is obtained.
It can be seen from the above examples that the process of the present invention can effectively remove impurities in hydrogen chloride gas, especially acetylene and ethylene impurities, to obtain electronic grade hydrogen chloride of 5N or more, and has the advantages of simple operation process, no need of additional reaction medium, and low production cost.
Claims (10)
1. A process for producingelectronic grade hydrogen chloride, wherein hydrogen chloride by-produced from petrochemical industry is used as a raw material, and impurities in the hydrogen chloride are separated and removed by a physical separation method, characterized by comprising the steps of reacting unsaturated hydrocarbons in the raw material with hydrogen chloride in the presence of a hydrochlorination catalyst, followed by separation and removal of the impurities.
2. The method according to claim 1, wherein the unsaturated hydrocarbon is acetylene, ethylene, and the acetylene is first subjected to a hydrochlorination reaction in the presence of an acetylene hydrochlorination catalyst, and the ethylene is subsequently subjected to a hydrochlorination reaction in the presence of an ethylene hydrochlorination catalyst.
3. The process according to claim 2, wherein the acetylene hydrochlorination catalyst has an acetylene conversion of not less than 95%, preferably not less than 99% under standard reaction conditions and the ethylene hydrochlorination catalyst has an ethylene conversion of not less than 95%, preferably not less than 99% under standard reaction conditions.
4. The method of claim 2 wherein the acetylene hydrochlorination catalyst is HgCl2-BaCl2/activated carbon composite catalyst in which BaCl2/HgCl20.1-0.5/1-2/10 of activated carbon, and CuCl as a catalyst for ethylene hydrochlorination2-KCl-SrCl2An active carbon composite catalyst, wherein the atomic ratio of Sr/K/Cu is 0.1-1.0/0.1-2/1, and CuCl2The weight ratio of the active carbon to the active carbon is 1-2.0/10.
5. The process according to claim 2, characterized in that the reaction conditions for the hydrochlorination of acetylene are: the pressure P is 0.1-7.0 MPa, the temperature T is 130-180 ℃, and the space velocity W of the raw materials is less than or equal to 90 kg/h.kg cat; operation strip for ethylene hydrochlorinationThe parts are as follows: the pressure is 0.1-7.0 MPa, the temperature T is 200-240 ℃, the space velocity of the raw material is less than or equal to 90 kg/h.kg cat, and O is optionally introduced into a deethylenizer reactor2In an amount of C2H4/O2＝1～2/1。
6. The process according to claim 2, characterized in that the raw material is subjected to a distillation process to remove impurities other than acetylene and ethylene from the hydrogen chloride before the hydrochlorination of acetylene and ethylene.
7. The method according to any one of claims 1 to 6, wherein the hydrogen chloride obtained through the previous round of the process of hydrochlorinating said unsaturated hydrocarbon with hydrogen chloride and separating off impurities is recycled to the hydrochlorination-separation process one or more times.
8. An apparatus for producing electronic grade hydrogen chloride, comprising a physical separation device, characterized in that it comprises a hydrochlorination reaction device for hydrochlorinating an unsaturated hydrocarbon contained in a raw hydrogen chloride with hydrogen chloride in the presence of a hydrochlorination catalyst, and an outlet of the hydrochlorination reaction device is connected to an inlet of the physical separation device.
9. The apparatus according to claim 8, wherein the hydrochlorination apparatus is an acetylene hydrochlorinationreactor and an ethylene hydrochlorination reactor, which are connected in series and are connected to a distillation/rectification and/or adsorption apparatus of the physical separation device.
10. The apparatus according to claim 8, characterized in that a light component removal distillation/rectification column and a heavy component removal distillation/rectification column are installed in sequence before the hydrochlorination reaction apparatus; and the outlet of the physical separation device is provided with a pipeline which is connected with the inlet of the hydrochlorination reaction device.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060271A (en) * | 2011-02-21 | 2011-05-18 | 上海正帆科技有限公司 | Method for producing electronic grade hydrochloric acid |
| CN107746040A (en) * | 2017-10-17 | 2018-03-02 | 山东新龙科技股份有限公司 | A kind of Processes and apparatus that hydrogen chloride is refined using the by-product gas for producing trichloro ethylene |
| CN108557766A (en) * | 2018-02-11 | 2018-09-21 | 浙江博瑞电子科技有限公司 | A kind of process for purification of hydrogen chloride |
| CN111268647A (en) * | 2020-04-15 | 2020-06-12 | 浙江博瑞电子科技有限公司 | Method for removing unsaturated fluorine-containing organic impurities in HCl |
| CN114634163A (en) * | 2022-05-18 | 2022-06-17 | 北京化工大学 | Production device and method for manufacturing electronic-grade hydrogen chloride |
-
2002
- 2002-12-31 CN CN 02159980 patent/CN1251964C/en not_active Expired - Lifetime
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060271A (en) * | 2011-02-21 | 2011-05-18 | 上海正帆科技有限公司 | Method for producing electronic grade hydrochloric acid |
| CN102060271B (en) * | 2011-02-21 | 2013-01-23 | 上海正帆科技有限公司 | Method for producing electronic grade hydrochloric acid |
| CN107746040A (en) * | 2017-10-17 | 2018-03-02 | 山东新龙科技股份有限公司 | A kind of Processes and apparatus that hydrogen chloride is refined using the by-product gas for producing trichloro ethylene |
| CN107746040B (en) * | 2017-10-17 | 2021-04-13 | 山东新龙科技股份有限公司 | Process and equipment for refining hydrogen chloride by using byproduct gas from production of trichloroethylene |
| CN108557766A (en) * | 2018-02-11 | 2018-09-21 | 浙江博瑞电子科技有限公司 | A kind of process for purification of hydrogen chloride |
| CN108557766B (en) * | 2018-02-11 | 2019-12-27 | 浙江博瑞电子科技有限公司 | Refining method of hydrogen chloride |
| CN111268647A (en) * | 2020-04-15 | 2020-06-12 | 浙江博瑞电子科技有限公司 | Method for removing unsaturated fluorine-containing organic impurities in HCl |
| CN114634163A (en) * | 2022-05-18 | 2022-06-17 | 北京化工大学 | Production device and method for manufacturing electronic-grade hydrogen chloride |
| CN114634163B (en) * | 2022-05-18 | 2022-08-05 | 北京化工大学 | Production device and method for manufacturing electronic grade hydrogen chloride |
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| CN1251964C (en) | 2006-04-19 |
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