CN114835086A - Hydrogen chloride gas purification technology - Google Patents
Hydrogen chloride gas purification technology Download PDFInfo
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- CN114835086A CN114835086A CN202210489906.9A CN202210489906A CN114835086A CN 114835086 A CN114835086 A CN 114835086A CN 202210489906 A CN202210489906 A CN 202210489906A CN 114835086 A CN114835086 A CN 114835086A
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 title claims abstract description 244
- 239000007789 gas Substances 0.000 title claims abstract description 140
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 229910000041 hydrogen chloride Inorganic materials 0.000 title claims abstract description 110
- 238000000746 purification Methods 0.000 title claims abstract description 28
- 238000005516 engineering process Methods 0.000 title claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 67
- 238000001035 drying Methods 0.000 claims abstract description 32
- 238000003795 desorption Methods 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002253 acid Substances 0.000 claims abstract description 11
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 129
- 238000003860 storage Methods 0.000 claims description 29
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 27
- 238000001179 sorption measurement Methods 0.000 claims description 27
- 238000012856 packing Methods 0.000 claims description 24
- 239000005416 organic matter Substances 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 18
- 239000000126 substance Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 229920006395 saturated elastomer Polymers 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 7
- 238000005507 spraying Methods 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 238000005984 hydrogenation reaction Methods 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 5
- 230000008929 regeneration Effects 0.000 claims description 5
- 238000011069 regeneration method Methods 0.000 claims description 5
- 230000001502 supplementing effect Effects 0.000 claims description 2
- KEQGZUUPPQEDPF-UHFFFAOYSA-N 1,3-dichloro-5,5-dimethylimidazolidine-2,4-dione Chemical compound CC1(C)N(Cl)C(=O)N(Cl)C1=O KEQGZUUPPQEDPF-UHFFFAOYSA-N 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 3
- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract 1
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 12
- 230000003647 oxidation Effects 0.000 description 6
- 238000007254 oxidation reaction Methods 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- -1 chloracyl Chemical compound 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000005660 chlorination reaction Methods 0.000 description 3
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 description 2
- 229940106681 chloroacetic acid Drugs 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/07—Purification ; Separation
- C01B7/0706—Purification ; Separation of hydrogen chloride
- C01B7/0718—Purification ; Separation of hydrogen chloride by adsorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention relates to a hydrogen chloride gas purification technology, which comprises the following steps: the method comprises the following steps: washing for the first time; step two: washing for the second time; step three: adsorbing organic matters; step four: absorbing acid preparation; step five: desorbing and drying; the hydrochloric acid as a byproduct is desorbed to obtain hydrogen chloride gas, primary washing and secondary washing are combined to recover organic matters in the gas, the hydrogen chloride gas is absorbed to prepare hydrochloric acid, and desorption drying is carried out to obtain relatively pure hydrogen chloride gas for a subsequent chlorosulfonic acid device.
Description
Technical Field
The invention relates to the technical field of chemical production, in particular to a hydrogen chloride gas purification technology.
Background
5 ten thousand tons/year chloroacetic acid apparatus for producing in the establishment of Jiangsutong's new material science and technology Limited company, the tail gas of chloroacetic acid is chlorination tail gas and two strands of gas of hydrogenation tail gas, contain a large amount of chlorine in the chlorination tail gas, contain a large amount of hydrogen in the hydrogenation tail gas, two strands of tail gas if incorporate one set of processing system, can produce the risk of explosion, so need separately handle two strands of materials, chlorination tail gas is as main process gas, get into clean system and handle, hydrogenation tail gas is because the volume is little relatively, can adopt original absorption system, prepare hydrochloric acid through the combination absorption tower, thereby separate out hydrogen, obtain about 7 ten thousand tons of 31% hydrochloric acid by-products.
The hydrochloric acid contains partial organic matters, so that the hydrochloric acid cannot be directly used and needs additional treatment, thereby increasing the environmental protection pressure of enterprises.
The organic matters in the hydrochloric acid are directly treated by adopting related processes such as rectification, desorption, absorption and the like, and the technology has certain difficulty, incomplete separation and high investment cost and operation cost.
Disclosure of Invention
The invention aims to provide a hydrogen chloride gas purification technology and solve the technical problem.
In order to solve the technical problems, the technical scheme of the invention is as follows: a hydrogen chloride gas purification technology is characterized in that hydrochloric acid prepared by a combined absorption tower is conveyed into a desorption system, and hydrogen chloride gas with the concentration of 80-90% is obtained by desorption, and the innovation points are as follows: further comprising the steps of:
the method comprises the following steps: primary washing: feeding hydrogen chloride gas into a primary washing tower for primary washing, wherein acetic acid with the concentration of 96-99.9% is continuously circulated in the primary washing tower;
step two: and (3) secondary washing: feeding the hydrogen chloride gas subjected to primary washing into a secondary washing tower for secondary washing, wherein concentrated hydrochloric acid which is circulated continuously is arranged in the secondary washing tower; the method is used for recovering organic matters in the gas, such as acetic acid, chloracyl, chlorine and acetic anhydride, by combining primary washing and secondary washing;
step three: organic matter adsorption: the hydrogen chloride gas after secondary washing is firstly sent into a hydrogen chloride cooler and a demister in sequence for cooling and demisting, and then sent into an organic matter adsorption purification device for removing trace organic matters contained in the hydrogen chloride gas; further removing residual organic matters in the gas;
step four: absorbing and preparing acid: feeding the hydrogen chloride gas without organic matters into 21% diluted acid to be absorbed to prepare 31% hydrochloric acid, and feeding tail gas containing non-condensable gas into an alkali absorption tower to be absorbed and purified and then to be discharged after reaching the standard;
step five: desorption and drying: preheating the obtained 31% hydrochloric acid, and then sending the preheated hydrochloric acid into a desorption tower for desorption to obtain hydrogen chloride gas, wherein the consumption of the 31% hydrochloric acid is 22-25 t/h; for desorbing hydrogen chloride in hydrochloric acid;
and then cooling the hydrogen chloride gas to 40-50 ℃ through primary condensation, cooling to about 5-12 ℃ through secondary condensation, and then sending the hydrogen chloride gas into a sulfuric acid drying system for drying to obtain hydrogen chloride gas with the concentration not less than 99.9%, so that the drying of the hydrogen chloride gas and the oxidation of trace organic matters are realized, the condensation is divided into two times, and the condensation effect is ensured.
Further, in the fifth step, the sulfuric acid drying system comprises a concentrated sulfuric acid storage tank, a dilute sulfuric acid storage tank, and a packed tower and a bubble cap packed tower which are connected in series, wherein sulfuric acid with the concentration not less than 98% and the temperature of 15-25 ℃ is filled in the concentrated sulfuric acid storage tank, and the dilute sulfuric acid storage tank is used for storing sulfuric acid with the concentration lower than 70%;
the concentrated sulfuric acid storage tank is communicated with the bubble cap packing tower through a liquid inlet pipeline and used for supplementing concentrated sulfuric acid into the bubble cap packing tower, the dilute sulfuric acid storage tank is connected with the bubble cap packing tower through a liquid discharge pipeline, an inlet of the liquid discharge pipeline is arranged at the bottom of the bubble cap packing tower, when the concentration of the sulfuric acid in the bubble cap packing tower is less than 70%, the dilute sulfuric acid is pumped into the dilute sulfuric acid storage tank for storage, the bubble cap packing tower and the bubble cap packing tower are communicated through a feeding pipeline and an air supply pipeline, an outlet of the feeding pipeline is arranged at the top of the bubble cap packing tower, the concentrated sulfuric acid in the bubble cap packing tower is conveyed into the top of the bubble cap packing tower through the feeding pipeline for spraying from top to bottom, and the hydrogen chloride gas after primary drying in the bubble cap packing tower is conveyed into the bubble cap packing tower through the air supply pipeline for secondary drying;
the packed tower is also connected with a sulfuric acid circulating pump and a sulfuric acid circulating cooler through a spraying circulating connecting pipe, the sulfuric acid in the packed tower is recycled by the sulfuric acid circulating pump, the temperature of the sulfuric acid is increased due to moisture absorption in the circulating process, and the sulfuric acid is cooled by the sulfuric acid cooler to improve the absorption efficiency;
the device comprises a packed tower, a circulating filter, a hydrogen chloride gas source, a circulating filter and a gas outlet, wherein the bottom of the packed tower is also provided with a gas inlet, the top of the packed tower is also provided with a gas outlet, the packed tower is also connected with the circulating filter, organic matters in the hydrogen chloride gas are oxidized by utilizing the characteristic that sulfuric acid has strong oxidation, and the oxidized organic matters are periodically discharged by adding the circulating filter.
Further, in the second step, substances which are dissolved with hydrochloric acid in the hydrogen chloride are washed by concentrated hydrochloric acid, the washed hydrochloric acid containing organic substances is sent to a hydrochloric acid storage tank, and periodically enters a conventional desorption system to desorb the hydrogen chloride, and is sent to a treatment system again to desorb the organic substances in the gas;
the hydrochloric acid can be treated regularly together with hydrochloric acid from hydrogenation reaction, so that the utilization rate is improved.
Furthermore, in the third step, after the organic matter in the organic matter adsorption and purification device is saturated, saturated steam is used for regeneration, continuous recycling is realized, the adsorption column is made of activated carbon fibers, the adsorption efficiency reaches more than 95%, and the adsorption time is 8 hours.
Furthermore, the flow speed of the hydrogen chloride gas is 2.5-3.5 t/h, and the high efficiency of the whole hydrogen chloride gas purification process is ensured.
The invention has the advantages that:
1) in the invention, the byproduct hydrochloric acid is desorbed to obtain hydrogen chloride gas, the primary washing and the secondary washing are combined to recover organic matters in the gas, the hydrochloric acid is prepared by absorption, and the relatively pure hydrogen chloride gas is obtained by desorption and drying and is used by a subsequent chlorosulfonic acid device.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a flow chart of a hydrogen chloride gas purification technique of the present invention.
Fig. 2 is a structural diagram of a sulfuric acid drying system according to the hydrogen chloride gas purification technique of the present invention.
Detailed Description
As shown in fig. 2, the sulfuric acid drying system of the hydrogen chloride gas purification technology includes a concentrated sulfuric acid storage tank 1, a dilute sulfuric acid storage tank 2, and a packed tower 3 and a bubble cap packed tower 4 connected in series, wherein the concentrated sulfuric acid storage tank 1 is filled with sulfuric acid with a concentration not less than 98%, and the dilute sulfuric acid storage tank 2 is used for storing sulfuric acid with a concentration less than 70%.
Concentrated sulfuric acid storage tank 1 and bubble cap packed tower 4 are through a liquid inlet pipeline intercommunication for mend concentrated sulfuric acid in 4 to bubble cap packed tower, dilute sulfuric acid storage tank 2 is connected through a drain pipe with packed tower 3, and the bottom of packed tower 3 is located to drain pipe's entry.
When the concentration of the sulfuric acid in the packed tower 3 is less than 70%, the dilute sulfuric acid is pumped into a dilute sulfuric acid storage tank 2 for storage, the packed tower 3 and the bubble cap packed tower 4 are communicated through a feeding pipeline 5 and an air supply pipeline 6, the outlet of the feeding pipeline 5 is arranged at the top of the packed tower 3, the concentrated sulfuric acid in the bubble cap packed tower 4 is conveyed into the top of the packed tower 3 through the feeding pipeline 5 for spraying from top to bottom, and the hydrogen chloride gas after primary drying in the packed tower 3 is conveyed into the bubble cap packed tower 4 through the air supply pipeline 6 for secondary drying.
The packed tower 3 is also connected with a sulfuric acid circulating pump 7 and a sulfuric acid circulating cooler 8 through a spraying circulating connecting pipe, the sulfuric acid in the packed tower 3 is recycled by the sulfuric acid circulating pump 7, the temperature of the sulfuric acid is increased due to moisture absorption in the circulating process, and the sulfuric acid is cooled by the sulfuric acid cooler to improve the absorption efficiency.
An air inlet has still been seted up to the bottom of packed tower 3, installs an intake pipe 9 for inside sending the hydrogen chloride gas into packed tower, a gas outlet has still been seted up at the top on the packed tower 3, packed tower 3 still is connected with a circulating filter 10, utilizes sulphuric acid to have strong oxidizing characteristic, oxidizes the organic matter in the hydrogen chloride gas, through increasing circulating filter 10, regularly discharges the organic matter after the oxidation.
As shown in figure 1, the hydrochloric acid produced by the combined absorption tower is conveyed into a desorption system and desorbed to obtain 86% hydrogen chloride gas.
Example I:
controlling the flow rate of the hydrogen chloride gas to be 2.5t/h, ensuring the high efficiency of the whole hydrogen chloride gas purification process, and then further comprising the following steps:
the method comprises the following steps: primary washing: feeding hydrogen chloride gas into a primary washing tower for primary washing, wherein acetic acid with the concentration of 99% is continuously circulated in the primary washing tower;
step two: and (3) secondary washing: feeding the hydrogen chloride gas subjected to primary washing into a secondary washing tower for secondary washing, wherein concentrated hydrochloric acid which is circulated continuously is arranged in the secondary washing tower; the method is used for recovering organic matters in the gas, such as acetic acid, chloracyl, chlorine and acetic anhydride, by combining primary washing and secondary washing;
in the second step, the concentrated hydrochloric acid is used for washing substances which are dissolved with the hydrochloric acid in the hydrogen chloride, the washed hydrochloric acid containing organic substances is sent to a hydrochloric acid storage tank, the hydrochloric acid periodically enters a conventional desorption system to desorb the hydrogen chloride, and the hydrogen chloride is sent to a treatment system again to remove the organic substances in the gas;
step three: organic matter adsorption: the hydrogen chloride gas after secondary washing is firstly sent into a hydrogen chloride cooler and a demister in sequence for cooling and demisting, and then sent into an organic matter adsorption purification device for removing trace organic matters contained in the hydrogen chloride gas; further removing residual organic matters in the gas;
after the organic matter in the organic matter adsorption and purification device is saturated, saturated steam is used for regeneration, continuous recycling is realized, the adsorption column is made of activated carbon fibers, and the adsorption time is 8 hours.
Step four: absorbing and preparing acid: feeding the hydrogen chloride gas without organic matters into 21% diluted acid to be absorbed to prepare 31% hydrochloric acid, and feeding tail gas containing non-condensable gas into an alkali absorption tower to be absorbed and purified and then to be discharged after reaching the standard;
step five: desorption and drying: preheating the obtained 31% hydrochloric acid, and then sending the preheated hydrochloric acid into a desorption tower for desorption to obtain hydrogen chloride gas, wherein the consumption of the 31% hydrochloric acid is 22 t/h;
and then cooling the hydrogen chloride gas to about 10 ℃, sending the hydrogen chloride gas into a sulfuric acid drying system, and drying the hydrogen chloride gas by using concentrated sulfuric acid with the temperature of 15 ℃ and the concentration of 98% to obtain the hydrogen chloride gas with the concentration of not less than 99.9%, thereby realizing the drying of the hydrogen chloride gas and the oxidation of trace organic matters.
Example II:
controlling the flow rate of the hydrogen chloride gas to be 3t/h, ensuring the high efficiency of the whole hydrogen chloride gas purification process, and then further comprising the following steps:
the method comprises the following steps: primary washing: feeding hydrogen chloride gas into a primary washing tower for primary washing, wherein acetic acid with the concentration of 99% is continuously circulated in the primary washing tower;
step two: and (3) secondary washing: feeding the hydrogen chloride gas subjected to primary washing into a secondary washing tower for secondary washing, wherein concentrated hydrochloric acid which is circulated continuously is arranged in the secondary washing tower; the method is used for recovering organic matters in the gas, such as acetic acid, chloracyl, chlorine and acetic anhydride, by combining primary washing and secondary washing;
in the second step, substances which are dissolved with hydrochloric acid in the hydrogen chloride are washed by concentrated hydrochloric acid, the washed hydrochloric acid containing organic substances is sent to a hydrochloric acid storage tank, and periodically sent to a conventional desorption system to desorb the hydrogen chloride, and then sent to a treatment system again to remove the organic substances in the gas;
step three: organic matter adsorption: the hydrogen chloride gas after secondary washing is firstly sent into a hydrogen chloride cooler and a demister in sequence for cooling and demisting, and then sent into an organic matter adsorption purification device for removing trace organic matters contained in the hydrogen chloride gas; further removing residual organic matters in the gas;
after the organic matter in the organic matter adsorption and purification device is saturated, saturated steam is used for regeneration, continuous recycling is realized, the adsorption column is made of activated carbon fibers, and the adsorption time is 8 hours.
Step four: absorbing and preparing acid: feeding the hydrogen chloride gas without organic matters into 21% diluted acid to be absorbed to prepare 31% hydrochloric acid, and feeding tail gas containing non-condensable gas into an alkali absorption tower to be absorbed and purified and then to be discharged after reaching the standard;
step five: desorption and drying: preheating the obtained 31% hydrochloric acid, and then sending the preheated hydrochloric acid into a desorption tower for desorption to obtain hydrogen chloride gas, wherein the consumption of the 31% hydrochloric acid is 23 t/h;
and then cooling the hydrogen chloride gas to about 10 ℃, sending the hydrogen chloride gas into a sulfuric acid drying system, and drying the hydrogen chloride gas by using concentrated sulfuric acid with the temperature of 20 ℃ and the concentration of 98% to obtain the hydrogen chloride gas with the concentration of not less than 99.9%, thereby realizing the drying of the hydrogen chloride gas and the oxidation of trace organic matters.
Example III:
controlling the flow rate of the hydrogen chloride gas to be 3.5t/h, ensuring the high efficiency of the whole hydrogen chloride gas purification process, and then further comprising the following steps:
the method comprises the following steps: primary washing: feeding hydrogen chloride gas into a primary washing tower for primary washing, wherein acetic acid with the concentration of 99% is continuously circulated in the primary washing tower;
step two: and (3) secondary washing: feeding the hydrogen chloride gas subjected to primary washing into a secondary washing tower for secondary washing, wherein concentrated hydrochloric acid which is circulated continuously is arranged in the secondary washing tower; the method is used for recovering organic matters in the gas, such as acetic acid, chloracyl, chlorine and acetic anhydride, by combining primary washing and secondary washing;
in the second step, the concentrated hydrochloric acid is used for washing substances which are dissolved with the hydrochloric acid in the hydrogen chloride, the washed hydrochloric acid containing organic substances is sent to a hydrochloric acid storage tank, the hydrochloric acid periodically enters a conventional desorption system to desorb the hydrogen chloride, and the hydrogen chloride is sent to a treatment system again to remove the organic substances in the gas;
step three: organic matter adsorption: the hydrogen chloride gas after secondary washing is firstly sent into a hydrogen chloride cooler and a demister in sequence for cooling and demisting, and then sent into an organic matter adsorption purification device for removing trace organic matters contained in the hydrogen chloride gas; further removing residual organic matters in the gas;
after the organic matter in the organic matter adsorption and purification device is saturated, saturated steam is used for regeneration, continuous recycling is realized, the adsorption column is made of activated carbon fibers, and the adsorption time is 8 hours.
Step four: absorbing and preparing acid: feeding the hydrogen chloride gas without organic matters into 21% diluted acid to be absorbed to prepare 31% hydrochloric acid, and feeding tail gas containing non-condensable gas into an alkali absorption tower to be absorbed and purified and then to be discharged after reaching the standard;
step five: desorption and drying: preheating the obtained 31% hydrochloric acid, and then sending the preheated hydrochloric acid into a desorption tower for desorption to obtain hydrogen chloride gas, wherein the consumption of the 31% hydrochloric acid is 25 t/h;
and then cooling the hydrogen chloride gas to about 10 ℃, sending the hydrogen chloride gas into a sulfuric acid drying system, and drying the hydrogen chloride gas by using concentrated sulfuric acid with the temperature of 25 ℃ and the concentration of 98% to obtain the hydrogen chloride gas with the concentration of not less than 99.9%, thereby realizing the drying of the hydrogen chloride gas and the oxidation of trace organic matters.
In conclusion:
the method can effectively remove the organic matters in the recovered gas, then the organic matters are absorbed to prepare hydrochloric acid, and the hydrochloric acid is desorbed and dried to obtain relatively pure hydrogen chloride gas for a subsequent chlorosulfonic acid device.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. A hydrogen chloride gas purification technology is characterized in that hydrochloric acid prepared by using a combined absorption tower is conveyed into a desorption system, and hydrogen chloride gas with the concentration of 80-90% is obtained by desorption, and the technology comprises the following steps: further comprising the steps of:
the method comprises the following steps: primary washing: feeding hydrogen chloride gas into a primary washing tower for primary washing, wherein acetic acid with the concentration of 96-99.9% is continuously circulated in the primary washing tower;
step two: and (3) secondary washing: feeding the hydrogen chloride gas subjected to primary washing into a secondary washing tower for secondary washing, wherein concentrated hydrochloric acid which is circulated continuously is arranged in the secondary washing tower;
step three: organic matter adsorption: the hydrogen chloride gas after secondary washing is firstly sent into a hydrogen chloride cooler and a demister in sequence for cooling and demisting, and then sent into an organic matter adsorption purification device for removing trace organic matters contained in the hydrogen chloride gas;
step four: absorbing and preparing acid: feeding the hydrogen chloride gas without organic matters into 21% diluted acid to be absorbed to prepare 31% hydrochloric acid, and feeding tail gas containing non-condensable gas into an alkali absorption tower to be absorbed and purified and then to be discharged after reaching the standard;
step five: desorption and drying: preheating the obtained 31% hydrochloric acid, and then sending the preheated hydrochloric acid into a desorption tower for desorption to obtain hydrogen chloride gas, wherein the consumption of the 31% hydrochloric acid is 22-25 t/h;
and cooling the hydrogen chloride gas to about 5-12 ℃, and then sending the hydrogen chloride gas into a sulfuric acid drying system for drying to obtain the hydrogen chloride gas with the concentration of not less than 99.9%.
2. The hydrogen chloride gas purification technology according to claim 1, wherein: in the fifth step, the sulfuric acid drying system comprises a concentrated sulfuric acid storage tank, a dilute sulfuric acid storage tank, and a packed tower and a bubble cap packed tower which are connected in series, wherein sulfuric acid with the concentration not less than 98% and the temperature of 15-25 ℃ is filled in the concentrated sulfuric acid storage tank, and the dilute sulfuric acid storage tank is used for storing sulfuric acid with the concentration lower than 70%;
the concentrated sulfuric acid storage tank is communicated with the bubble cap packing tower through a liquid inlet pipeline and used for supplementing concentrated sulfuric acid into the bubble cap packing tower, the dilute sulfuric acid storage tank is connected with the bubble cap packing tower through a liquid discharge pipeline, an inlet of the liquid discharge pipeline is arranged at the bottom of the bubble cap packing tower, when the concentration of the sulfuric acid in the bubble cap packing tower is less than 70%, the dilute sulfuric acid is pumped into the dilute sulfuric acid storage tank for storage, the bubble cap packing tower and the bubble cap packing tower are communicated through a feeding pipeline and an air supply pipeline, an outlet of the feeding pipeline is arranged at the top of the bubble cap packing tower, the concentrated sulfuric acid in the bubble cap packing tower is conveyed into the top of the bubble cap packing tower through the feeding pipeline for spraying from top to bottom, and the hydrogen chloride gas after primary drying in the bubble cap packing tower is conveyed into the bubble cap packing tower through the air supply pipeline for secondary drying;
the packed tower is also connected with a sulfuric acid circulating pump and a sulfuric acid circulating cooler through a spraying circulating connecting pipe, the sulfuric acid in the packed tower is recycled by the sulfuric acid circulating pump, the temperature of the sulfuric acid is increased due to moisture absorption in the circulating process, and the sulfuric acid is cooled by the sulfuric acid cooler to improve the absorption efficiency;
the device comprises a packed tower, a gas inlet, a gas outlet, a circulating filter, a gas inlet, a gas outlet, a gas inlet, a gas outlet, a circulating filter, a gas outlet, a gas inlet, a gas outlet.
3. The hydrogen chloride gas purification technique according to claim 1, wherein: in the second step, the concentrated hydrochloric acid is used for washing substances which are dissolved with the hydrochloric acid in the hydrogen chloride, the washed hydrochloric acid containing organic substances is sent to a hydrochloric acid storage tank, the hydrochloric acid periodically enters a conventional desorption system to desorb the hydrogen chloride, and the hydrogen chloride is sent to a treatment system again to remove the organic substances in the gas;
this hydrochloric acid may be periodically treated together with the hydrochloric acid from the hydrogenation.
4. The hydrogen chloride gas purification technique according to claim 1, wherein: in the third step, after the organic matter in the organic matter adsorption and purification device is saturated, saturated steam is used for regeneration, continuous recycling is realized, the adsorption column is made of activated carbon fibers, the adsorption efficiency reaches more than 95%, and the adsorption time is 8 hours.
5. The hydrogen chloride gas purification technique according to claim 1, wherein: the flow velocity of the hydrogen chloride gas is 2.5-3.5 t/h.
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| CN109319739A (en) * | 2018-11-30 | 2019-02-12 | 南通星球石墨设备有限公司 | A kind of hydrogen chloride drying system and drying means |
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| CN1433958A (en) * | 2002-01-25 | 2003-08-06 | 黑龙江齐化化工有限责任公司 | Process for purifying hydrogen chloride |
| JP2010189206A (en) * | 2009-02-16 | 2010-09-02 | Mitsui Chemicals Inc | Method for producing chlorine |
| CN102816045A (en) * | 2012-09-05 | 2012-12-12 | 河北科技大学 | Method for synthesizing chloromethane by tail gas generated during chloroacetic acid production |
| CN109319739A (en) * | 2018-11-30 | 2019-02-12 | 南通星球石墨设备有限公司 | A kind of hydrogen chloride drying system and drying means |
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Application publication date: 20220802 |