CN115650173A - Preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of R134A device - Google Patents
Preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of R134A device Download PDFInfo
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- CN115650173A CN115650173A CN202211361553.0A CN202211361553A CN115650173A CN 115650173 A CN115650173 A CN 115650173A CN 202211361553 A CN202211361553 A CN 202211361553A CN 115650173 A CN115650173 A CN 115650173A
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Abstract
The invention discloses a preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of an R134A device, which comprises the following steps: step one, taking TCE and AHF as raw materials, carrying out fluorination reaction on the TCE and the AHF in a reactor according to a certain ratio to generate R134A, separating a byproduct of HCL through a rectifying tower, separating high-purity HCl from the top of the tower, decompressing the HCL gas to normal pressure through a flow meter regulating valve, and then feeding the HCL gas into a washing tower, controlling the temperature of the top of the separating tower to be-35 to-25 ℃, controlling the pressure to be 0.9 to 1.1Mpa, and controlling the temperature difference to be 0 to 5 ℃; step two, in the washing of a washing tower, some metal ions in HCL gas are washed away and then enter an absorber together with acid below a tail gas tower; the preparation method disclosed by the invention has the advantages that the preparation process of producing the electronic-grade hydrochloric acid by producing the byproduct HCL of the R134A device is simple, the operation is convenient, the generation of waste water can be effectively reduced, a large amount of steam and electric power can be effectively reduced, the resources are effectively saved, the operation cost is reduced, the product preparation purity can be effectively improved, and the impurity removal effect is good.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of an R134A device.
Background
TCE and AHF are used as raw materials in the production of the R134A device, the TCE and the AHF are subjected to fluorination reaction in a reactor according to a certain proportion to generate R134A, a byproduct is HCL, HCL is separated through a rectifying tower, and is separated from the top of the tower, wherein the HCL contains 50ppm of HF,50ppm of organic matters and 20ppm of free chlorine. At present, 31% of industrial hydrochloric acid is adopted for purification of electronic-grade hydrochloric acid, and the purification mainly comprises a rectification method, a distillation method, a sub-boiling distillation method and the like, and the industrial production of the electronic-grade hydrochloric acid is mainly prepared by a continuous rectification method, so that a large amount of steam and electric power are consumed, and the generation amount of wastewater is large.
Disclosure of Invention
The invention aims to provide a preparation method for producing electronic-grade hydrochloric acid by using HCL as a byproduct of an R134A device, which has the advantages of simple preparation process for producing the electronic-grade hydrochloric acid by using HCL as the byproduct of the R134A device, convenient operation, effective reduction of waste water generation, effective reduction of a large amount of steam and electric power, effective resource saving, operation cost reduction, effective improvement of product preparation purity and good impurity removal effect.
The purpose of the invention can be realized by the following technical scheme:
the preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of R134A device comprises the following steps:
step one, taking TCE and AHF as raw materials, carrying out fluorination reaction on the TCE and the AHF in a reactor according to a certain ratio to generate R134A, separating a byproduct of HCL through a rectifying tower, separating high-purity HCl from the top of the tower, decompressing the HCL gas to normal pressure through a flow meter regulating valve, and then feeding the HCL gas into a washing tower, controlling the temperature of the top of the separating tower to be-35 to-25 ℃, controlling the pressure to be 0.9 to 1.1Mpa, and controlling the temperature difference to be 0 to 5 ℃;
step two, in washing of a washing tower, after some metal ions in HCL gas are washed away, the metal ions and the acid under the tail gas tower enter an absorber;
and step three, absorbing the HCL gas and the low-concentration hydrochloric acid from the bottom of the tail gas tower in the absorber, allowing the qualified electronic-grade hydrochloric acid at the bottom of the absorber to enter a hydrochloric acid storage tank, and allowing the incompletely absorbed HCL gas to enter the tail gas tower.
As a further scheme of the invention: in the third step, in the tail gas tower, ultrapure water/steam condensate water in the high-level water tank washes the tail gas which is not completely absorbed by the absorber again through the second flowmeter and the second regulating valve.
As a further scheme of the invention: in the third step, indexes such as free chlorine, metal ions and the like of ultrapure water/steam condensate water in the high-level water tank must meet the requirement of electronic-grade hydrochloric acid.
As a further scheme of the invention: in the third step, the tail gas tower is made of steel lining PTFE, and the filler is PTFE pall ring filler.
As a further scheme of the invention: in the first step, the washing tower is made of lining PTFE, the operating pressure is 0-60 kPa, and the operating temperature is-25-80 ℃.
As a further scheme of the invention: in the second step, the absorber is a circular hole block type graphite falling film absorber, the operation pressure is 0-60 kPa, and the operation temperature is 25-80 ℃.
The invention has the beneficial effects that: the preparation method disclosed by the invention has the advantages that the preparation process of producing the electronic-grade hydrochloric acid by producing the byproduct HCL of the R134A device is simple, the operation is convenient, the generation of waste water can be effectively reduced, a large amount of steam and electric power can be effectively reduced, the resources are effectively saved, the operation cost is reduced, the product preparation purity can be effectively improved, the impurity removal effect is good, and the method is worthy of wide popularization and application.
Drawings
In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.
FIG. 1 is a process flow diagram of the present invention;
in the figure: 1. a separation column; 2. a first flow meter; 3. a first regulating valve; 4. a washing tower; 5. an absorber; 6. a circulation pump; 7. a tail gas tower; 8. a hydrochloric acid storage tank; 9. a high-level water tank; 10. a second flow meter; 11. a second regulating valve.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1, the preparation method of electronic-grade hydrochloric acid by byproduct HCL of R134A device comprises the following steps:
step one, taking TCE and AHF as raw materials, carrying out fluorination reaction on the TCE and the AHF in a reactor according to a certain ratio to generate R134A, taking HCl as a byproduct, separating 1 through a rectifying tower, separating high-purity HCl from the top of the tower, decompressing the HCL gas to normal pressure through a first flowmeter 2 and a second regulating valve 3, and allowing the HCL gas to enter a washing tower, wherein the temperature of the top of the separating tower 1 is controlled to be-35 ℃ to-25 ℃, the pressure is controlled to be 0.9-1.1 MPa, and the temperature difference is controlled to be 0-5 ℃; the washing tower 4 is made of lining PTFE, the operating pressure is 0-60 kPa, and the operating temperature is-25-80 ℃;
step two, in the washing of a washing tower 4, after washing away some metal ions in HCL gas, the metal ions and acid under a tail gas tower 7 enter an absorber 5; the absorber 5 is a circular hole block type graphite falling film absorber, the operation pressure is 0-60 kPa, and the operation temperature is 25-80 ℃;
absorbing HCL gas and low-concentration hydrochloric acid from the bottom of a tail gas tower 7 in an absorber 5, feeding qualified electronic-grade hydrochloric acid from the bottom of the absorber 5 into a hydrochloric acid storage tank 8, and feeding HCL gas which is not completely absorbed into the tail gas tower 7; the tail gas tower 7 is made of steel lining PTFE, and the filler is PTFE pall ring filler; indexes such as free chlorine, metal ions and the like of the ultrapure water/steam condensate water in the high-level water tank 9 must meet the requirement of electronic grade hydrochloric acid; in the tail gas tower 7, the ultrapure water/steam condensed water in the high-level water tank 9 is used for washing the tail gas which is not completely absorbed by the absorber again through a second flowmeter 10 and a second regulating valve 11.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (6)
- A preparation method for producing electronic-grade hydrochloric acid from byproduct HCL of an R134A device is characterized by comprising the following steps:step one, taking TCE and AHF as raw materials, carrying out fluorination reaction on the TCE and the AHF in a reactor according to a certain proportion to generate R134A, taking HCl as a byproduct, separating the HCL through a rectifying tower, separating high-purity HCl from the top of the tower, decompressing HCL gas to normal pressure through a flow meter regulating valve, and then feeding the HCL gas into a washing tower, controlling the temperature of the top of the separating tower to be-35 to-25 ℃, controlling the pressure to be 0.9 to 1.1Mpa, and controlling the temperature difference to be 0 to 5 ℃;step two, in washing of a washing tower, after some metal ions in HCL gas are washed away, the metal ions and the acid under the tail gas tower enter an absorber;and step three, absorbing the HCL gas and low-concentration hydrochloric acid from the bottom of the tail gas tower in an absorber, allowing qualified electronic-grade hydrochloric acid at the bottom of the absorber to enter a hydrochloric acid storage tank, and allowing the HCL gas which is not completely absorbed to enter the tail gas tower.
- 2. The method for preparing electronic-grade hydrochloric acid from HCL as a byproduct of the R134A device according to claim 1, wherein in the third step, the tail gas which is not completely absorbed by the absorber is washed again by the ultrapure water/steam condensed water in the high-level water tank through the second flowmeter and the second regulating valve in the tail gas tower.
- 3. The method for preparing electronic-grade hydrochloric acid by-product HCL of R134A device according to claim 1, wherein in the third step, indexes such as free chlorine and metal ions of ultrapure water/steam condensate water in the high-level water tank must meet requirements of electronic-grade hydrochloric acid.
- 4. The method for preparing electronic-grade hydrochloric acid by producing HCL as a byproduct of the R134A device according to claim 2, wherein in the third step, the material of the tail gas tower is steel-lined PTFE, and the filler is PTFE pall ring filler.
- 5. The method for preparing electronic-grade hydrochloric acid by-product HCL production of an R134A device according to claim 1, wherein in the first step, the washing tower is made of lining PTFE, the operating pressure is 0-60 kPa, and the operating temperature is-25 ℃ to 80 ℃.
- 6. The method for preparing electronic-grade hydrochloric acid by-product HCL production of the R134A device according to claim 1, wherein in the second step, the absorber is a round-hole block type graphite falling film absorber, the operating pressure is 0-60 kPa, and the operating temperature is 25-80 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211361553.0A CN115650173A (en) | 2022-11-02 | 2022-11-02 | Preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of R134A device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211361553.0A CN115650173A (en) | 2022-11-02 | 2022-11-02 | Preparation method for producing electronic-grade hydrochloric acid by using byproduct HCL of R134A device |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017191388A1 (en) * | 2016-05-03 | 2017-11-09 | Arkema France | Hydrochloric acid purification process and plant |
| CN108017039A (en) * | 2017-12-24 | 2018-05-11 | 江苏梅兰化工有限公司 | Monochlorodifluoromethane by-product HCL produces the preparation method and device of high purity hydrochloric acid |
| CN109761196A (en) * | 2019-03-01 | 2019-05-17 | 江苏梅兰化工有限公司 | A kind of method for producing electronic grade hydrochloric acid |
| WO2022127018A1 (en) * | 2020-12-16 | 2022-06-23 | 浙江天采云集科技股份有限公司 | Ftrpsa separation and purification method for refinement of electronic-grade hf from industrial-grade high-concentration hf |
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2022
- 2022-11-02 CN CN202211361553.0A patent/CN115650173A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017191388A1 (en) * | 2016-05-03 | 2017-11-09 | Arkema France | Hydrochloric acid purification process and plant |
| CN108017039A (en) * | 2017-12-24 | 2018-05-11 | 江苏梅兰化工有限公司 | Monochlorodifluoromethane by-product HCL produces the preparation method and device of high purity hydrochloric acid |
| CN109761196A (en) * | 2019-03-01 | 2019-05-17 | 江苏梅兰化工有限公司 | A kind of method for producing electronic grade hydrochloric acid |
| WO2022127018A1 (en) * | 2020-12-16 | 2022-06-23 | 浙江天采云集科技股份有限公司 | Ftrpsa separation and purification method for refinement of electronic-grade hf from industrial-grade high-concentration hf |
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