CN114956949A - Hydrochloric acid resolving and recycling process - Google Patents
Hydrochloric acid resolving and recycling process Download PDFInfo
- Publication number
- CN114956949A CN114956949A CN202210721231.6A CN202210721231A CN114956949A CN 114956949 A CN114956949 A CN 114956949A CN 202210721231 A CN202210721231 A CN 202210721231A CN 114956949 A CN114956949 A CN 114956949A
- Authority
- CN
- China
- Prior art keywords
- sulfuric acid
- hydrochloric acid
- amount
- evaporation
- dilute
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
- C07C17/16—Preparation of halogenated hydrocarbons by replacement by halogens of hydroxyl groups
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention belongs to the field of hydrochloric acid analysis and recovery, in particular to a hydrochloric acid analysis and recovery process, which aims at solving the problem that the existing hydrochloric acid is inconvenient to analyze and provides the following scheme, comprising the following steps: s1, mixing dilute hydrochloric acid and concentrated sulfuric acid; s2, transferring water in the dilute hydrochloric acid to concentrated sulfuric acid to form dilute sulfuric acid, and then, carrying out hydrogenolysis on the chlorination; s3, sending the resolved hydrogen chloride to a hydrochlorination reactor, and reacting the hydrogen chloride with vaporized methanol under the action of a catalyst to generate a crude methane chloride product; s4, removing impurities and drying the crude product, sending the crude product to a compression process, and cooling the compressed methane chloride and storing the cooled methane chloride in a storage tank; s5, evaporating and dehydrating the dilute sulfuric acid, concentrating the dilute sulfuric acid into concentrated sulfuric acid for recycling, condensing evaporated water to obtain acidic wastewater, and metering the acidic wastewater.
Description
Technical Field
The invention relates to the technical field of hydrochloric acid desorption and recovery, in particular to a hydrochloric acid desorption and recovery process.
Background
In the production process of methane chloride, hydrogen chloride tail gas is generated, and the hydrogen chloride tail gas is absorbed by water to produce a byproduct of 31% hydrochloric acid which is totally sold in the market, so that the following risks exist at present: due to the influence of the large environment, the market demand rate of the byproduct hydrochloric acid is lower and lower, the byproduct hydrochloric acid is always sold in a lost state, the storage capacity of a production workshop is large, and the environmental protection risk of a company is large; the leakage risk is large in the process of selling and transporting the byproduct hydrochloric acid, if the byproduct hydrochloric acid leaks into a water body, the leakage can cause great environmental protection influence, and therefore the hydrochloric acid needs to be analyzed and recycled.
In the prior art, hydrochloric acid is inconvenient to resolve, so a hydrochloric acid resolving and recycling process is provided for solving the problems.
Disclosure of Invention
The invention aims to solve the problem that hydrochloric acid is inconvenient to analyze in the prior art, and provides a hydrochloric acid analyzing and recycling process.
In order to achieve the purpose, the invention adopts the following technical scheme:
a hydrochloric acid resolving and recycling process comprises the following steps:
s1, mixing dilute hydrochloric acid and concentrated sulfuric acid;
s2, transferring water in the dilute hydrochloric acid to concentrated sulfuric acid to form dilute sulfuric acid, and then carrying out hydrogenolysis on the chlorination;
s3, sending the resolved hydrogen chloride to a hydrochlorination reactor, and reacting the hydrogen chloride with vaporized methanol under the action of a catalyst to generate a crude methane chloride product;
s4, removing impurities and drying the crude product, sending the crude product to a compression process, and cooling the compressed methane chloride and storing the cooled methane chloride in a storage tank;
s5, evaporating and dehydrating dilute sulfuric acid, concentrating the dilute sulfuric acid into concentrated sulfuric acid for recycling, condensing evaporated water to obtain acidic wastewater, and metering the acidic wastewater;
s6, metering dilute sulfuric acid before evaporation through a metering device;
and S7, measuring the amount of sulfuric acid after the evaporation is finished, calculating the evaporation amount, comparing the calculated evaporation amount with the collected amount of the acidic wastewater, and judging whether leakage exists or not.
Preferably, in S1, dilute hydrochloric acid is measured, concentrated sulfuric acid is measured according to the amount of the dilute hydrochloric acid, and the measured concentrated sulfuric acid is added to the dilute hydrochloric acid and mixed by an analytical tower.
Preferably, in S5, dilute sulfuric acid is added into a sealed heating container, and the dilute sulfuric acid is heated by the sealed heating container, wherein the heating temperature is 130 ℃.
Preferably, the steam generated by heating the sealed heating container is introduced into the cooling cavity, and the steam is cooled and recovered by the cooler.
Preferably, the cooled and recovered liquid is neutralized with an alkaline neutralizing agent, the pH value of the liquid is detected by a pH value detector after neutralization, and the liquid is discharged after qualified detection.
Preferably, in S7, the amount of sulfuric acid is measured after completion of the evaporation, the evaporation amount is calculated, the calculated evaporation amount is compared with the amount of the collected acidic wastewater, and if the amount of the collected acidic wastewater is lower than the evaporation amount and the lower amount exceeds a predetermined value, a possibility of leakage is indicated.
Preferably, in S5, the temperature controller detects the temperature during evaporation and transmits the detected data to the control center.
Preferably, in S4, the crude product is purified by a rectifying tower and then dried by concentrated sulfuric acid.
Compared with the prior art, the invention has the beneficial effects that:
the method removes the coalescence phase of the carbon-oxygen alkane in the dilute hydrochloric acid, and the carbon-oxygen alkane in the acid can be controlled to be reduced to below 50PPm, thereby providing guarantee for the long-period operation of hydrochloric acid analysis; concentrated sulfuric acid is used as a boiling breaking agent, the dilution heat of the concentrated sulfuric acid is fully utilized, and meanwhile, the concentrated sulfuric acid is continuously added from the top of the analysis tower, so that the reflux ratio of the top of the analysis tower is reduced to the minimum, the energy consumption is saved to the maximum extent, and the steam consumption is low;
the amount of sulfuric acid is measured after evaporation is finished, the evaporation amount is calculated, and the calculated evaporation amount is compared with the amount of the collected acidic wastewater, so that whether leakage occurs or not can be judged;
the invention is convenient for analyzing and recovering the hydrochloric acid and can judge whether the recovery process leaks or not.
Drawings
Fig. 1 is a flow chart of a hydrochloric acid resolving and recycling process provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
Referring to fig. 1, a hydrochloric acid desorption and recovery process includes the following steps:
s1, mixing dilute hydrochloric acid and concentrated sulfuric acid;
s2, transferring water in the dilute hydrochloric acid to concentrated sulfuric acid to form dilute sulfuric acid, and then, carrying out hydrogenolysis on the chlorination;
s3, sending the resolved hydrogen chloride to a hydrochlorination reactor, and reacting the hydrogen chloride with vaporized methanol under the action of a catalyst to generate a crude methane chloride product;
s4, removing impurities and drying the crude product, sending the crude product to a compression process, and cooling the compressed methane chloride and storing the cooled methane chloride in a storage tank;
s5, evaporating and dehydrating the dilute sulfuric acid, concentrating the dilute sulfuric acid into concentrated sulfuric acid for recycling, condensing evaporated water to obtain acidic wastewater, and metering the acidic wastewater;
s6, metering dilute sulfuric acid before evaporation through a metering device;
and S7, measuring the amount of sulfuric acid after the evaporation is finished, calculating the evaporation amount, comparing the calculated evaporation amount with the collected amount of the acidic wastewater, and judging whether leakage exists or not.
In this embodiment, dilute hydrochloric acid is measured, concentrated sulfuric acid is measured according to the amount of the dilute hydrochloric acid, and the measured concentrated sulfuric acid is added to the dilute hydrochloric acid and stirred while being added, wherein the stirring speed is 100r/min, and the stirring time is 10 min.
In this embodiment, dilute sulfuric acid is added to a sealed heating container, and the dilute sulfuric acid is heated by the sealed heating container at a heating temperature of 100 ℃.
In this embodiment, the steam that the heating of sealed heating container produced lets in the cooling chamber, cools off the recovery through the cooler to steam.
In this embodiment, the cooled and recovered liquid is neutralized with an alkaline neutralizing agent, the PH value of the liquid is detected by a PH value detector after neutralization, and the liquid is discharged after being detected to be qualified.
In this example, the amount of sulfuric acid was measured after evaporation was completed, the amount of evaporation was calculated, the calculated amount of evaporation was compared with the amount of collected acidic wastewater, and if the amount of collected acidic wastewater was less than the amount of evaporation and the amount of evaporation less than the expected value, it indicated that there was a possibility of leakage.
In this embodiment, during evaporation and dehydration, the temperature during evaporation is detected by the temperature controller, and the detected data is transmitted to the control center.
In this embodiment, the crude product is purified by a rectifying tower, and then dried by concentrated sulfuric acid.
Example two
Referring to fig. 1, a hydrochloric acid desorption and recovery process includes the following steps:
s1, mixing dilute hydrochloric acid and concentrated sulfuric acid;
s2, transferring water in the dilute hydrochloric acid to concentrated sulfuric acid to form dilute sulfuric acid, and then, carrying out hydrogenolysis on the chlorination;
s3, sending the resolved hydrogen chloride to a hydrochlorination reactor, and reacting the hydrogen chloride with vaporized methanol under the action of a catalyst to generate a crude methane chloride product;
s4, removing impurities and drying the crude product, sending the crude product to a compression process, and cooling the compressed methane chloride and storing the cooled methane chloride in a storage tank;
s5, evaporating and dehydrating dilute sulfuric acid, concentrating the dilute sulfuric acid into concentrated sulfuric acid for recycling, condensing evaporated water to obtain acidic wastewater, and metering the acidic wastewater;
s6, metering dilute sulfuric acid before evaporation through a metering device;
and S7, measuring the amount of sulfuric acid after the evaporation is finished, calculating the evaporation amount, comparing the calculated evaporation amount with the collected amount of the acidic wastewater, and judging whether leakage exists or not.
In this example, dilute hydrochloric acid was measured, concentrated sulfuric acid was measured according to the amount of the dilute hydrochloric acid, and the measured concentrated sulfuric acid was added to the dilute hydrochloric acid while stirring, with a stirring speed of 150r/min and a stirring time of 12 min.
In this embodiment, dilute sulfuric acid is added to a sealed heating container, and the dilute sulfuric acid is heated by the sealed heating container at a temperature of 110 ℃.
In this embodiment, the steam that the heating of sealed heating container produced lets in the cooling chamber, cools off the recovery through the cooler to steam.
In this embodiment, the cooled and recovered liquid is neutralized with an alkaline neutralizing agent, the PH value of the liquid is detected by a PH value detector after neutralization, and the liquid is discharged after being detected to be qualified.
In this embodiment, the amount of sulfuric acid is measured after evaporation is completed, the amount of evaporation is calculated, the calculated amount of evaporation is compared with the amount of collected acidic wastewater, and if the amount of collected acidic wastewater is lower than the amount of evaporation and the lower amount exceeds an expected value, it is indicated that there is a possibility of leakage.
In the embodiment, during evaporation and dehydration, the temperature during evaporation is detected through the temperature controller, and the detected data is transmitted to the control center.
In this embodiment, the crude product is purified by a rectifying tower, and then dried by concentrated sulfuric acid.
EXAMPLE III
Referring to fig. 1, a hydrochloric acid desorption and recovery process includes the following steps:
s1, mixing dilute hydrochloric acid and concentrated sulfuric acid;
s2, transferring water in the dilute hydrochloric acid to concentrated sulfuric acid to form dilute sulfuric acid, and then, carrying out hydrogenolysis on the chlorination;
s3, sending the resolved hydrogen chloride to a hydrochlorination reactor, and reacting the hydrogen chloride with vaporized methanol under the action of a catalyst to generate a crude methane chloride product;
s4, removing impurities and drying the crude product, sending the crude product to a compression process, and cooling the compressed methane chloride and storing the cooled methane chloride in a storage tank;
s5, evaporating and dehydrating the dilute sulfuric acid, concentrating the dilute sulfuric acid into concentrated sulfuric acid for recycling, condensing evaporated water to obtain acidic wastewater, and metering the acidic wastewater;
s6, metering dilute sulfuric acid before evaporation through a metering device;
and S7, measuring the amount of sulfuric acid after the evaporation is finished, calculating the evaporation amount, comparing the calculated evaporation amount with the collected amount of the acidic wastewater, and judging whether leakage exists or not.
In this example, dilute hydrochloric acid was measured, concentrated sulfuric acid was measured according to the amount of the dilute hydrochloric acid, and the measured concentrated sulfuric acid was added to the dilute hydrochloric acid and stirred while being added, with a stirring speed of 200r/min and a stirring time of 15 min.
In this embodiment, dilute sulfuric acid is added to a sealed heating container, and the dilute sulfuric acid is heated by the sealed heating container at a temperature of 120 ℃.
In this embodiment, the steam that the heating of sealed heating container produced lets in the cooling chamber, cools off the recovery through the cooler to steam.
In this embodiment, the cooled and recovered liquid is neutralized with an alkaline neutralizing agent, the PH value of the liquid is detected by a PH value detector after neutralization, and the liquid is discharged after being detected to be qualified.
In this example, the amount of sulfuric acid was measured after evaporation was completed, the amount of evaporation was calculated, the calculated amount of evaporation was compared with the amount of collected acidic wastewater, and if the amount of collected acidic wastewater was less than the amount of evaporation and the amount of evaporation less than the expected value, it indicated that there was a possibility of leakage.
In this embodiment, during evaporation and dehydration, the temperature during evaporation is detected by the temperature controller, and the detected data is transmitted to the control center.
In this embodiment, the crude product is purified by a rectifying tower, and then dried by concentrated sulfuric acid.
Through the hydrochloric acid analyzing and recycling process provided by the first, second and third embodiments, the hydrochloric acid can be analyzed and recycled conveniently, and meanwhile, whether leakage occurs in the recycling process can be judged, and the second embodiment is the best embodiment.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The hydrochloric acid resolving and recycling process is characterized by comprising the following steps of:
s1, mixing dilute hydrochloric acid and concentrated sulfuric acid;
s2, transferring water in the dilute hydrochloric acid to concentrated sulfuric acid to form dilute sulfuric acid, and then, carrying out hydrogenolysis on the chlorination;
s3, sending the resolved hydrogen chloride to a hydrochlorination reactor, and reacting the hydrogen chloride with vaporized methanol under the action of a catalyst to generate a crude methane chloride product;
s4, removing impurities and drying the crude product, sending the crude product to a compression process, and cooling the compressed methane chloride and storing the cooled methane chloride in a storage tank;
s5, evaporating and dehydrating the dilute sulfuric acid, concentrating the dilute sulfuric acid into concentrated sulfuric acid for recycling, condensing evaporated water to obtain acidic wastewater, and metering the acidic wastewater;
s6, metering dilute sulfuric acid before evaporation through a metering device;
and S7, measuring the amount of sulfuric acid after the evaporation is finished, calculating the evaporation amount, comparing the calculated evaporation amount with the collected amount of the acidic wastewater, and judging whether leakage exists or not.
2. The process of claim 1, wherein in S1, dilute hydrochloric acid is measured, concentrated sulfuric acid is measured according to the amount of dilute hydrochloric acid, the measured concentrated sulfuric acid is added to the dilute hydrochloric acid and stirred at a stirring speed of 100-.
3. The analytic recovery process of hydrochloric acid as claimed in claim 1, wherein in S5, dilute sulfuric acid is added into the sealed heating container, and the diluted sulfuric acid is heated by the sealed heating container at a temperature of 100 ℃ to 120 ℃.
4. The analytic recovery process of hydrochloric acid of claim 3, wherein the steam generated by heating the sealed heating container is introduced into a cooling chamber, and the steam is cooled and recovered by a cooler.
5. The analytic recovery process of hydrochloric acid as in claim 4, wherein the cooled recovered liquid is neutralized with an alkaline neutralizing agent, and after neutralization, the pH value of the liquid is detected by a pH value detector, and the liquid is discharged after passing the detection.
6. The analytical recovery process for hydrochloric acid as claimed in claim 1, wherein in S7, the amount of sulfuric acid is measured after completion of evaporation, the amount of evaporation is calculated, the calculated amount of evaporation is compared with the amount of collected acidic wastewater, and if the amount of collected acidic wastewater is less than the amount of evaporation and the amount of evaporation is more than the expected amount, it indicates the possibility of leakage.
7. The process of claim 1, wherein in step S5, the temperature during evaporation is detected by a temperature controller during evaporation and dehydration, and the detected data is transmitted to a control center.
8. The analytical recovery process of hydrochloric acid as claimed in claim 1, wherein in S4, the crude product is purified by a rectifying tower and then dried by concentrated sulfuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210721231.6A CN114956949A (en) | 2022-06-24 | 2022-06-24 | Hydrochloric acid resolving and recycling process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210721231.6A CN114956949A (en) | 2022-06-24 | 2022-06-24 | Hydrochloric acid resolving and recycling process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114956949A true CN114956949A (en) | 2022-08-30 |
Family
ID=82966529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210721231.6A Pending CN114956949A (en) | 2022-06-24 | 2022-06-24 | Hydrochloric acid resolving and recycling process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114956949A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440015A (en) * | 2008-11-27 | 2009-05-27 | 山东东岳氟硅材料有限公司 | Method for producing methane chloride by using dilute hydrochloric acid |
-
2022
- 2022-06-24 CN CN202210721231.6A patent/CN114956949A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101440015A (en) * | 2008-11-27 | 2009-05-27 | 山东东岳氟硅材料有限公司 | Method for producing methane chloride by using dilute hydrochloric acid |
Non-Patent Citations (1)
| Title |
|---|
| 王勇等: "硫酸法盐酸深解吸装置在有机硅行业的应用", 有机硅材料, vol. 36, no. 3, pages 65 - 68 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107188133B (en) | Device and method for separating sucralose tail gas | |
| CN109336803B (en) | Method and system for recovering production solvent from NMP waste liquid | |
| CN106362548A (en) | Treating method of oxidized tail gas in process of manufacturing cyclohexanone with cyclohexane oxidation method | |
| CN114031056A (en) | Method for preparing phosphorus pentafluoride by polymerizing phosphate | |
| CN105645358A (en) | Method for preparing hydrogen fluoride from fluosilicic acid | |
| CN110683519A (en) | Method and device for treating lithium hexafluorophosphate synthesis tail gas | |
| CN210356586U (en) | Tail gas recovery equipment for process for preparing lithium hexafluorophosphate by anhydrous hydrogen fluoride solvent method | |
| CN103482650A (en) | Equipment for preparing ammonium fluoride or ammonium bifluoride by adopting fluosilicic acid and liquid ammonia and production method | |
| CN102617273B (en) | Method for producing trichlorotrifluoroethane by high-temperature gas phase chlorination method | |
| CN101440015A (en) | Method for producing methane chloride by using dilute hydrochloric acid | |
| CN114956949A (en) | Hydrochloric acid resolving and recycling process | |
| CN103816768B (en) | From producing the method and system reclaiming hydrogen chloride chloromethanes or tetrachloro-ethylene tail gas | |
| CN103342399A (en) | Stripping system and stripping method for cleaning waste sodium hypochlorite in production of acetylene by virtue of calcium carbide method | |
| CN207445913U (en) | Epoxychloropropane chlorination workshop section tail gas absorbing system | |
| CN110041299A (en) | A kind of method that the continuous gas phase catalytic fluorination of fixed bed prepares fluorinated ethylene carbonate | |
| CN103708993B (en) | A kind of vinylidene is thick cracking gas alkali cleaning and dehydrating process in producing | |
| CN111499490B (en) | Method for producing chloromethane by using byproduct fluorine-containing hydrogen chloride | |
| CN102103105A (en) | Novel method for measuring Kjeldahl nitrogen | |
| CN113321193B (en) | Method for recovering nitric acid from nitric acid waste liquid | |
| CN211813429U (en) | Device for preparing hydrogen chloride by using sulfur-based compound fertilizer waste acid | |
| CN104262623B (en) | Polyphenylene sulfide material crystal vulcanized sodium rectification under vacuum dehydrating process | |
| CN107827085B (en) | Process and equipment for continuously preparing sulfur dioxide by fuming sulfuric acid | |
| CN112537814A (en) | Treatment system for fluorine-containing nitric acid waste liquid | |
| CN203437120U (en) | Deamination and dehydration device for sodium persulfate (persulfate) synthetic fluid | |
| CN103848721A (en) | Aldehyde removal apparatus of pentaerythritol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |