CN1311053A - Refining and recovering process for industrial by-product halogen hydride gas - Google Patents
Refining and recovering process for industrial by-product halogen hydride gas Download PDFInfo
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- CN1311053A CN1311053A CN 00103388 CN00103388A CN1311053A CN 1311053 A CN1311053 A CN 1311053A CN 00103388 CN00103388 CN 00103388 CN 00103388 A CN00103388 A CN 00103388A CN 1311053 A CN1311053 A CN 1311053A
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Abstract
The present invention relates to the refining and recovery technology of by product hydrogen halide gas. In said technology, the byproduct hydrogen halide gas enters from the tower bottom and contacts with the circulating washing solvent, such as concentrated hydrochloric acid, countercurrent in the tower from the tower top, then it is reacted, dissolved and washed to remove the impurities in HCl gas. The rofined HCl gas comes out from the tower top and enters into the absorption system and absorbed by water to form hydrochloric acid product.
Description
Often be accompanied by the generation of a large amount of by-product hydrogen halide gases in organic and inorganic chemical industry are produced, industrial often water absorption or neutralization are handled simply.Because hydrogen halides produces in course of reaction, gas phase can be carried a certain amount of raw material, product intermediate and accessory substance secretly, and the acid that water absorption by-product hydrogen halide obtains can only be worked as spent acid and be handled the transfer that pollutes and the waste of resource.
The refining common treating method of by-product hydrogen halide is to remove high-boiling components with shell and tube condenser cooling earlier.Because mass transfer is insufficient, gas flow rate is big, and heat-transfer effect is bad, and the impurity of carrying secretly can not Ex-all, can not fundamentally solve the refining problem of hydrogen halides.Some factory adopts many still series connection, improves raw material availability, because gas flow is big, the gas-liquid contact is insufficient, DeGrain.Contain 10% organic impurities in the hydrogen chloride tail gas as by-product in the production processes of chloroacetic acid.
And most of systems have the certain vacuum degree, and perhaps the tail gas outlet pressure is lower, thereby adopt the fluid-tight mode to allow gas pass liquid layer and realize that absorption is restricted.A kind ofly will be of great importance if invent at the general hydrogen halide refining plant of most of system.Moreover, if can be reduced to the impurity in the hydrogen halide below 0.1%, then can make full use of the hydrogen halides resource, the change spent acid is useful industrial acid, even reagent acid, thereby alleviates the deficiency of domestic chlorine, bromine resource.
Disclose the method for many refining hydrochloric acid in the prior art, for example, US 4,786, and 488 disclose and a kind ofly put forward the method that the hydrochloric acid of a carbon chlorohydrocarbon impurity comes purifying hydrochloric acid with HCl gas gas.In this patent, being intended to hydrochloric acid liquid that gas carries enters the tower of filling concentrated hydrochloric acid liquid from the top of bubble tower packed bed, and at the bottom of tower, hydrochloric acid is heated to boiling by evaporimeter, generation is used for the HCl gas that gas is carried chlorohydrocarbon, described HCl gas is with chlorohydrocarbon, upwards, discharge, and the hydrochloric acid that gas was carried takes out at the bottom of tower from cat head by bubble tower.But this method is not suitable for direct purification gaseous by-product hydrogen halides, the refining hydrochloric acid that obtains.
The present invention is based in the hydrogen halide most of organic and inorganic impurity can be dissolved in the respective media, or its raw material or intermediate can and be trapped with the respective media reaction, for example in the monoxone tail gas except containing HCl, also contain vinegar acyl chlorides, chloracetyl chloride, S
2Cl
2, they can generate acetic acid and monoxone with water reaction, separate out sulphur, generate HCl simultaneously, and hydrogen halide has sizable boiling-point difference with these medium solutions, have proposed the employing tower and have made with extra care hydrogen halides.
Against vacuum and pressure-fired system, it is suitable adopting the packed tower rectification flow, for example refining technological process of the present invention that can adopt as shown in Figure 1 of by-product hydrogen chloride gas in the production processes of chloroacetic acid.
Process description:
1. the impure HCl gas that comes out by production system, entering from HCl treating column 1 bottom, is 10-60 ℃ in the tower temperature, is preferably in 20-40 ℃ the tower and the circulation cleaning solvent counter current contacting that enters from cat head, by reaction, dissolving and washing, remove most of impurity contained in the HCl gas.
2. the HCl gas behind the primary purification, come out from HCl treating column 1 top, utilize pressure reduction, enter HCl treating column 2 from the bottom, in temperature is 10-60 ℃, be preferably in 20-40 ℃ the tower and the circulation cleaning solvent counter current contacting in tower that enters from cat head,, thoroughly remove impurity contained in the HCl gas by reaction, dissolving and washing.HCl gas after refining is made finished product hydrochloric acid by the cat head extraction to the absorption of absorption system water.
3. the circulation cleaning solvent adopts saturated hydrochloric acid.Earlier saturated hydrochloric acid is joined in the circulating tank 4, carry through circulating pump 6, remove mechanical admixture contained in the circulating solvent and gel, floccule through piping filter 8, regulate flows through flowmeter 10 again, add, contact with up HCl back flow of gas at Ta Nei from HCl treating column 2 tops, remove impurity contained in the HCl gas, the circulation cleaning solvent that has dissolved impurity goes out from tower bottom flow, gets back to circulating tank 4, and then recycles.
4. when the impurity in the circulating tank 4 reaches finite concentration (acetic acid, monoxone concentration reach 10%-30%) possibly can't thoroughly remove the impurity in the HCl gas again.At this moment, the circulating solvent in the circulating tank 4 is carried through pump 6, changed in the circulating tank 3,, replenish new saturated hydrochloric acid in the circulating tank 4 again as the circulating solvent of HCl treating column 1 by pipeline 11 (among the figure shown in the dotted line).
5. the circulating solvent in the circulating tank 3 is carried and piping filter 7 filtrations through circulating pump 5, and carries by flowmeter 9, enters from HCl treating column 1 top, and the circulation cleaning solvent that has dissolved impurity goes out from tower bottom flow, gets back to circulating tank 3, and then recycles.Be recycled to impurity content and reach finite concentration (decide according to the system situation, its limiting case is that the water in the hydrochloric acid all reacts with vinegar acyl chlorides, chloracetyl chloride, generates corresponding acetic acid and monoxone), discharge turns back to production system or handles as spent acid.
Also can circulation type gas purification tower mode, for example, the byproduct hydrogen chloride tail gas that produces when producing chlroacetone for the dyestuff factory can adopt technological process of the present invention as shown in Figure 2.
Process description:
1. the impure HCl gas that comes out by production system, enter through the micropore distributor from the circulation flow reactor bottom, in temperature is 10-60 ℃, be preferably in 20-40 ℃ the reactor and the circulation cleaning solvent counter current contacting that enters from the reactor napex, by reaction, dissolving and washing, thoroughly remove impurity contained in the HCl gas.
2. the HCl gas after refining comes out from the circulation flow reactor top, and to the HCl absorption system, and the circulation cleaning solvent comes out to get back to the circulating tank from the circulation flow reactor bottom.
HCl gas purification tower of the present invention adopts continuous multi-stage countercurrent equipment (plate column) or Continuous Contact adverse current equipment (packed tower).
It is that gas and cleaning solvent can realize repeatedly washing balance at Ta Nei that the present invention adopts the foundation of tower equipment, the filler of certain altitude can be equivalent to the washing of tens grades even tens grades, guaranteed that impurity reacts with the circulation cleaning solvent fully and is dissolved in the circulation cleaning solvent, thereby impurity has been removed to greatest extent.
By the tower height of selecting to suit, can make reaction carry out obtaining qualified refining hydrogen chloride gas at cat head fully, the hydrogen chloride gas after making with extra care absorbs through gas absorbing device and obtains elaboration hydrochloric acid.
The reaction of gas in tower, according to the separate sources of gas, the circulation cleaning solvent of its mechanism and employing is also different.With the monoxone by-product hydrogen chloride gas is example, made full use of the reaction of water (or water vapour) with acyl chlorides, chloracetyl chloride, sulfur dichloride, contact by the continuous flow upstream of water with production of chloroacetic acid tail gas, vinegar acyl chlorides in the tail gas, chloracetyl chloride and water reaction are generated acetic acid and monoxone, be dissolved in the water and enrichment, and then recycled.Sulfur dichloride and water reaction generation sulphur is removed through piping filter in the tail gas.
Gas source among the present invention can be the hydrogen halide of production process by-product, also can be the hydrogen halide that the spent acid after the absorption obtains through gasification.
The circulation cleaning solvent that the present invention mentions can be water, acetic acid, raw material, product or higher is arranged, and easily dissolves other solvent of impurity in the hydrogen halide.Circulation cleaning solvent as the refining employing of by-product hydrogen chloride in the production of chloroacetic acid can be water, watery hydrochloric acid, saturated hydrochloric acid or acetic acid, preferred saturated hydrochloric acid.The hydrogen chloride useful raw materials of by-product or product such as benzene, chlorobenzene equal solvent wash refining in the chlorobenzene production process.
The material of tower adopts corresponding resistant material according to the characteristic of different systems among the present invention.Filler in the tower is all kinds filler of acid corrosion-resistant, and the height of filler is generally 2 to 20 meters, and concrete height is decided according to condition such as pressure, tolerance, gas speed and the refining quality that will reach of system.
The mode that can adopt single tower also can adopt multitower series connection or tower to connect among the present invention with still, the circulation cleaning solvent is single medium during single-tower rectifying, the circulation cleaning solvent that adopts multitower series connection or tower and still series system to adopt is multiple medium.
The hydrogen halide treating column adopts continuous multi-stage countercurrent equipment (plate column) or Continuous Contact adverse current equipment (packed tower), and outlet has the system of higher malleation also can adopt the tower or water conservancy diversion cartridge type gas purification tower of bubbling for tail gas.
Temperature during purification operations of the present invention is lower than the boiling point of cleaning solvent, generally with material non-crystallizable and energy-conservation be principle, can suitably reduce operating temperature.
Below adopt the mode of embodiment that the present invention is carried out non-limiting explanation.
Making with extra care of [industrial implementation example 1] monoxone tail gas by-product hydrochloric acid
Adopt technological process of the present invention shown in Figure 1 that tail gas in the production of chloroacetic acid is carried out refinement treatment.Contain impurity such as acetic acid, chloracetyl chloride, vinegar acyl chlorides and sulfur dichloride in the handled monoxone tail gas, the about 2-5% of content.During refinement treatment, the inlet amount of HCl gas is controlled at 50-100 liter/second, and the diameter for the treatment of column 1,2 is 500mm, and temperature is 20-30 ℃ in the tower, and the circulation cleaning solvent is saturated hydrochloric acid, its flow-control the 1000-1200 liter/hour.Refining through two-stage, the content of hydrochloric acid of gained is 36.5%, and in the HCl total acid, the purity of hydrochloric acid is 99.85%, and organic impurity content is less than 0.1%.The refining hydrochloric acid water white transparency that obtains reaches the industrial synthesis hydrochloric acid standard.
By-product hydrochloric acid is refining in [industrial implementation example 2] chlroacetone production process
Adopt technological process of the present invention shown in Figure 2 that HCl tail gas in the chlroacetone production is carried out refinement treatment.Contain acetone, monochloroacetone and dichloroacetone (1,1-dichloroacetone and 1,3-dichloroacetone) in the handled accessory substance HCl tail gas, the about 2-3% of its content.During refinement treatment, HCl gas feed amount is controlled at 500 liters/minute, and the temperature of circulation flow reactor is 20-30 ℃, and the circulation flow reactor diameter is 400mm, and the circulation cleaning solvent is saturated hydrochloric acid, its flow-control the 15-20 liter/minute.After refining, the purity of the refining hydrochloric acid of gained reaches 99.9%, and organic impurity content reaches the industrial synthesis hydrochloric acid quality less than 0.1%.Adopting circulation type gas purification tower shown in the accompanying drawing 2, is cleaning solvent with saturated hydrochloric acid, and the purity of the refining hydrochloric acid of gained reaches 99.9%, and organic impurity content reaches the industrial synthesis hydrochloric acid quality less than 0.1%.
Making with extra care of [industrial implementation example 3] dimethylphosphite by-product hydrochloric acid
Adopt technological process of the present invention shown in Figure 1 that HCl gas in the dimethylphosphite production is carried out refinement treatment.Contain impurity such as phosphorus trichloride, methyl alcohol, chloromethyl ester and dimethylphosphite, the about 3-8% of content in the handled dimethylphosphite by-product HCl gas.During refinement treatment, the inlet amount of HCl gas is controlled at 100-200 liter/second, and the diameter for the treatment of column 1,2 is 700mm, and temperature is 20-30 ℃ in the tower, and the circulation cleaning solvent is saturated hydrochloric acid, its flow-control the 2000-2400 liter/hour.Refining through two-stage, the content of hydrochloric acid of gained is 36.5%, and in the HCl total acid, the purity of hydrochloric acid is 99.9%, and organic impurity content is less than 0.1%.The refining hydrochloric acid water white transparency that obtains reaches the industrial synthesis hydrochloric acid standard.
Claims (10)
1. the method for by-product hydrogen halide gas in the refining chemical process, it is characterized in that by-product hydrogen halide gas feeds at the bottom of by tower, with the circulation cleaning solvent counter current contacting in tower that enters from cat head, by reaction, dissolving and washing, remove the impurity that contains in the HCl gas, the circulation cleaning solvent goes out from tower bottom flow, recycles, and the HCl gas after refining is by the cat head extraction, enter absorption system, water absorbs, and makes finished product hydrochloric acid.
2. according to the process of claim 1 wherein, the source of described hydrogen halide can be a production process by-product hydrogen halide gas, also can be the hydrogen halide that the spent acid after absorbing obtains through gasification.
3. according to the process of claim 1 wherein the mode of the single tower of refining employing of described hydrogen halide or multitower series connection, still series connection.
4. according to the method for claim 3, wherein, when adopting single-tower rectifying, the circulation cleaning solvent is single medium.
5. according to the method for claim 3, wherein, when adopting multitower series connection or tower to connect with still, the circulation cleaning solvent is single or the multimedium system.
6. according to the process of claim 1 wherein, described hydrogen halide treating column adopts continuous multi-stage countercurrent equipment, for example plate column, perhaps Continuous Contact adverse current equipment, for example packed tower.
7. according to the process of claim 1 wherein, when the tail gas outlet has the system of higher malleation, adopt the tower or water conservancy diversion cartridge type gas purification tower of bubbling.
8. according to the process of claim 1 wherein, described circulation cleaning solvent is water, halogen acids, raw material, product or higher is arranged, and easily dissolves other solvent of impurity in the hydrogen halide.
9. according to the process of claim 1 wherein, the operating temperature of described hydrogen halide treating column is 10-60 ℃.
10. according to the process of claim 1 wherein, the material of described hydrogen halide treating column is a resistant material, and inner-tower filling material is all kinds filler of acid corrosion-resistant, and the height of filler is 2 to 20 meters.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00103388A CN1130246C (en) | 2000-03-03 | 2000-03-03 | Refining and recovering process for industrial by-product halogen hydride gas |
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|---|---|---|---|
| CN00103388A CN1130246C (en) | 2000-03-03 | 2000-03-03 | Refining and recovering process for industrial by-product halogen hydride gas |
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| CN1311053A true CN1311053A (en) | 2001-09-05 |
| CN1130246C CN1130246C (en) | 2003-12-10 |
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| CN00103388A Expired - Fee Related CN1130246C (en) | 2000-03-03 | 2000-03-03 | Refining and recovering process for industrial by-product halogen hydride gas |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101274195B (en) * | 2007-12-24 | 2010-06-30 | 天津大学 | Method for removing residual chlorine gas in tail gas in production processes of chloroacetic acid |
| CN101185835B (en) * | 2007-08-23 | 2010-08-18 | 周滢 | Method for absorbing and using waste gases hydrogen chloride produced in chemical industrial products |
| CN101870457A (en) * | 2010-06-29 | 2010-10-27 | 蓝星化工有限责任公司 | Method for purifying by-product hydrogen chloride gas of TDI |
| CN101648104B (en) * | 2008-08-13 | 2011-06-22 | 北京格瑞华阳科技发展有限公司 | Technology for reclaiming hydrogen chloride tail gas in chemical production |
| CN102849681A (en) * | 2012-04-06 | 2013-01-02 | 昊华鸿鹤化工有限责任公司 | Method for removing chlorine included in hydrogen chloride gas |
| CN105480948A (en) * | 2015-12-16 | 2016-04-13 | 南京工业大学 | Method and system for recycling by-product hydrogen chloride in fatty acid or fatty acyl chloride chlorination production process |
| CN106310875A (en) * | 2015-07-01 | 2017-01-11 | 启东久星化工有限公司 | System for separating organic matter from mixture of hydrogen chloride and organic matter |
| CN106621427A (en) * | 2016-12-08 | 2017-05-10 | 张贵 | Cold evaporation purifying system for by-product hydrochloric acid |
| CN107043090A (en) * | 2017-01-06 | 2017-08-15 | 江苏吉华化工有限公司 | It is a kind of to be used to improve the devices and methods therefor for reclaiming removal rate of sulfur dioxide in hydrochloric acid |
| CN108310912A (en) * | 2017-01-18 | 2018-07-24 | 湖北星火化工有限公司 | A kind of processing unit of hydrochloric acid tank tail gas |
| CN114262258A (en) * | 2021-12-23 | 2022-04-01 | 浙江万盛股份有限公司 | Method for resource preparation of dichloropropanol from impurity-containing phosphate flame retardant industrial byproduct HCl |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3207887A1 (en) * | 1982-03-05 | 1983-09-15 | Chemische Werke Hüls AG, 4370 Marl | METHOD FOR PURIFYING SALT ACIDS |
| US4629610A (en) * | 1985-05-10 | 1986-12-16 | Dow Chemical Co. | Hydrogen fluoride recovery process |
| US5352420A (en) * | 1989-04-17 | 1994-10-04 | Krc Umwelttechnik Gmbh | Process for the purification of waste gas having a high chloride content |
| WO1998002402A1 (en) * | 1996-07-17 | 1998-01-22 | Texaco Development Corporation | Method for minimizing hydrogen halide corrosion in a partial oxidation process |
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- 2000-03-03 CN CN00103388A patent/CN1130246C/en not_active Expired - Fee Related
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101185835B (en) * | 2007-08-23 | 2010-08-18 | 周滢 | Method for absorbing and using waste gases hydrogen chloride produced in chemical industrial products |
| CN101274195B (en) * | 2007-12-24 | 2010-06-30 | 天津大学 | Method for removing residual chlorine gas in tail gas in production processes of chloroacetic acid |
| CN101648104B (en) * | 2008-08-13 | 2011-06-22 | 北京格瑞华阳科技发展有限公司 | Technology for reclaiming hydrogen chloride tail gas in chemical production |
| CN101870457A (en) * | 2010-06-29 | 2010-10-27 | 蓝星化工有限责任公司 | Method for purifying by-product hydrogen chloride gas of TDI |
| CN101870457B (en) * | 2010-06-29 | 2011-12-28 | 蓝星化工有限责任公司 | Method for purifying by-product hydrogen chloride gas of TDI |
| CN102849681A (en) * | 2012-04-06 | 2013-01-02 | 昊华鸿鹤化工有限责任公司 | Method for removing chlorine included in hydrogen chloride gas |
| CN106310875A (en) * | 2015-07-01 | 2017-01-11 | 启东久星化工有限公司 | System for separating organic matter from mixture of hydrogen chloride and organic matter |
| CN105480948A (en) * | 2015-12-16 | 2016-04-13 | 南京工业大学 | Method and system for recycling by-product hydrogen chloride in fatty acid or fatty acyl chloride chlorination production process |
| CN105480948B (en) * | 2015-12-16 | 2018-05-18 | 南京工业大学 | A kind of aliphatic acid or fat acyl chloride chlorination production byproduct in process object hydrogen chloride circulation utilization method and system |
| CN106621427A (en) * | 2016-12-08 | 2017-05-10 | 张贵 | Cold evaporation purifying system for by-product hydrochloric acid |
| CN107043090A (en) * | 2017-01-06 | 2017-08-15 | 江苏吉华化工有限公司 | It is a kind of to be used to improve the devices and methods therefor for reclaiming removal rate of sulfur dioxide in hydrochloric acid |
| CN107043090B (en) * | 2017-01-06 | 2019-08-06 | 江苏吉华化工有限公司 | It is a kind of for improve recycling hydrochloric acid in removal rate of sulfur dioxide devices and methods therefor |
| CN108310912A (en) * | 2017-01-18 | 2018-07-24 | 湖北星火化工有限公司 | A kind of processing unit of hydrochloric acid tank tail gas |
| CN114262258A (en) * | 2021-12-23 | 2022-04-01 | 浙江万盛股份有限公司 | Method for resource preparation of dichloropropanol from impurity-containing phosphate flame retardant industrial byproduct HCl |
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| Publication number | Publication date |
|---|---|
| CN1130246C (en) | 2003-12-10 |
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Owner name: BEIJING ZIGUANG YING LI CHEMICAL TECHNOLOGY CO., L Free format text: FORMER NAME: QINGHUAZIGUANG YINGLI CHEMICAL TECHNOLOGY CO. LTD., BEIJING |
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Address after: No. 18 Anning East Road, Beijing, Haidian District Patentee after: TH-UNIS Insight Co., Ltd. Address before: Room 506, purple building, Tsinghua University, Beijing Patentee before: Beijing Tsinghua Unisplendour Insight Chemical Technology LLC |
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Granted publication date: 20031210 Termination date: 20100303 |