CN101219943A - Method for purifying and using chloroethanoic acid tail gas - Google Patents
Method for purifying and using chloroethanoic acid tail gas Download PDFInfo
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- CN101219943A CN101219943A CNA2007100001413A CN200710000141A CN101219943A CN 101219943 A CN101219943 A CN 101219943A CN A2007100001413 A CNA2007100001413 A CN A2007100001413A CN 200710000141 A CN200710000141 A CN 200710000141A CN 101219943 A CN101219943 A CN 101219943A
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- tail gas
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- concentrated sulfuric
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Abstract
The invention relates to a method for purifying and utilizing chloroactic acid tail gas, which adopts segmented cooling and condensation and concentrated sulfuric acid washing to purify and utilizes tail gas produced in chloroactic acid production, which can not only recycle most of the raw materials and chloride intermediate but also make the gas into hydrochloride or high-purity hydrogen chloride meeting an industrial standard. The method is characterized in that the condition of segmented cooling and condensation is to cool the tail gas to 0 DEG C to minus 20 DEG C, the optimum condition is minus 10 DEG C to minus 20 DEG C, the condition of the concentrated sulfuric acid washing is to use concentrated sulfuric acid of 93 percent to 98 percent, the optimum condition is to use concentrated sulfuric acid of 95 percent to 98 percent. Simultaneously, the method also solves the environmental pollution problem caused by the chloroactic acid tail gas, which generates a certain economical benefit and social benefit.
Description
Technical field
The present invention relates to Chloroethanoic acid tail gas purifying and utilize method, belong to fine chemistry industry environmental protection field.
Background technology
Adopt acetic acid chlorination method to produce in the chloroacetic process, one ton of Mono Chloro Acetic Acid of every production will produce the hydrogen chloride gas about 400 kilograms, because exhaust gas component complexity, can not be directly used in the production of other Chemicals, therefore, domestic most of producers only absorb into the tail gas water by-product hydrochloric acid about 30% at present, undersell to the metal processing industry as spent acid, for acid pickling and rust removing usefulness, or as the spent acid neutralizing treatment.
Chinese patent CN1837175A discloses improving one's methods of preparation process for chloroacetic acid, allow the tail gas of gases such as containing hydrogenchloride, acetic acid, Mono Chloro Acetic Acid, acyl chlorides, sulfur subchloride, before entering the absorption tower, at first enter the resorber that hydrochloric acid is housed in, the acetic acid that has in the tail gas, Mono Chloro Acetic Acid, acyl chlorides, sulfur subchloride are reclaimed a part, be recovered acid, add again as raw material and catalyzer and proceed reaction in the reactor.Be to have reclaimed part material and chlorination intermediate like this, but the share that reclaims is very limited, only be about 3% of acetic acid consumption quota, and still contain the chlorination intermediate of severe overweight in final absorption is made about 30% the hydrochloric acid, be still seriously polluted underproof spent acid.
Summary of the invention
The objective of the invention is to reclaim as far as possible acetic acid and chlorination intermediate in the tail gas; And make hydrochloric acid or exsiccant purity higher (＞99%) hydrogen chloride gas that meets industrial synthetic hydrochloric acid standard.
Technical scheme of the present invention is: the tail gas that contains acetic acid and chlorination intermediate from chlorination reaction still gas-liquid separator comes out, enter two placed in-line cooler condensers, and separate acid solution with entering separator after the cooling of underground water and chilled brine respectively.Enter then to be filled with and be soaked with organosilyl beta glass fibre strainer, send into vitriol oil washer after removing acid mist, after the tail gas after the vitriol oil washing is removed acid mist, promptly obtain the purer hydrogen chloride gas of exsiccant; This gas absorbs through water and just makes industrial hydrochloric acid.The condition of segmentation cooling condensation is that tail gas is cooled to 0 ℃～-20 ℃.Optimal conditions is-10 ℃～-20 ℃; The condition of vitriol oil washing is that vitriol oil concentration is 93%～98%, and optimal conditions is 95%～98%.
Effect of the present invention is after adopting above-mentioned technology: can reclaim raw material and the chlorination intermediate of acetic acid consumption quota more than 10%; And make the hydrochloric acid that meets industrial synthetic acidity scale standard.Solve problem of environmental pollution simultaneously, produced favorable economic benefit and social benefit.
Embodiment
Embodiment one
Mono Chloro Acetic Acid tail gas is water-cooled to 25 ℃ with underground earlier; Be cooled to 0 ℃ with-5 ℃～-10 ℃ chilled brines again, merge phlegma, analyze its composition and be: chloroacetyl chloride 10% (weight), Acetyl Chloride 98Min. 30～40% (weight), acetic acid, Mono Chloro Acetic Acid, sulfur subchlorides etc. 35～45% the rest is hydrochloric acid.
Embodiment two
With above-mentioned tail gas through two sections cooling condensations, the dry hydrogen chloride after washing is collected in the vitriol oil washing with 98%, analyzes it and consists of: chloracetyl acid content (weight):＞99%, and water-content (weight):＜0.02%.Last water absorbs, and makes high purity hydrochloric acid, and analytical results is: hydrogen chloride content % (weight): 33%, and H
2SO
4Content is (with SO
4 2-Meter, * 10
-6)＜1, and free chlorine content (in Cl-, * 10
-6)＜1, CH
3OOH, and chloracetyl, Mono Chloro Acetic Acid etc. do not detect.
Claims (1)
1. a Chloroethanoic acid tail gas purifying and utilize method.The method that adopts the segmentation cooling condensation and the vitriol oil to wash purifies and utilizes the tail gas of production of chloroacetic acid, most raw materials and chlorination intermediate have not only been reclaimed, also tail gas is made the hydrochloric acid or the high-purity hydrogen chloride gas that meet industrial synthetic hydrochloric acid standard, it is characterized in that: the condition of segmentation cooling condensation is that tail gas is cooled to 0 ℃～-20 ℃, optimal conditions is-10 ℃～-20 ℃, the condition of vitriol oil washing is the vitriol oil with 93%～98%, and optimal conditions is 95%～98% the vitriol oil.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100001413A CN101219943A (en) | 2007-01-08 | 2007-01-08 | Method for purifying and using chloroethanoic acid tail gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007100001413A CN101219943A (en) | 2007-01-08 | 2007-01-08 | Method for purifying and using chloroethanoic acid tail gas |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101219943A true CN101219943A (en) | 2008-07-16 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007100001413A Pending CN101219943A (en) | 2007-01-08 | 2007-01-08 | Method for purifying and using chloroethanoic acid tail gas |
Country Status (1)
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|---|---|
| CN (1) | CN101219943A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036080A (en) * | 2015-07-28 | 2015-11-11 | 江苏同泰化工有限公司 | Method for preparing high-concentration refined hydrochloric acid by using tail gas hydrogen chloride generated from chloroacetic acid production |
| CN105060249A (en) * | 2015-07-28 | 2015-11-18 | 江苏同泰化工有限公司 | Method for preparing refined hydrochloric acid by using tail gas hydrogen chloride produced in chloroacetic acid production |
| CN105129734A (en) * | 2015-07-28 | 2015-12-09 | 江苏同泰化工有限公司 | Method for recovering available substances in chloroacetic acid production tail gas |
| CN106000075A (en) * | 2016-07-08 | 2016-10-12 | 浙江闰土新材料有限公司 | Method and device for purifying, absorbing and recycling chlorinated gas in benzene chlorination process |
-
2007
- 2007-01-08 CN CNA2007100001413A patent/CN101219943A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036080A (en) * | 2015-07-28 | 2015-11-11 | 江苏同泰化工有限公司 | Method for preparing high-concentration refined hydrochloric acid by using tail gas hydrogen chloride generated from chloroacetic acid production |
| CN105060249A (en) * | 2015-07-28 | 2015-11-18 | 江苏同泰化工有限公司 | Method for preparing refined hydrochloric acid by using tail gas hydrogen chloride produced in chloroacetic acid production |
| CN105129734A (en) * | 2015-07-28 | 2015-12-09 | 江苏同泰化工有限公司 | Method for recovering available substances in chloroacetic acid production tail gas |
| CN105036080B (en) * | 2015-07-28 | 2017-06-16 | 江苏同泰化工有限公司 | The method that the refined hydrochloric acid of high concentration is prepared using the tail gas hydrogen chloride for producing monoxone generation |
| CN106000075A (en) * | 2016-07-08 | 2016-10-12 | 浙江闰土新材料有限公司 | Method and device for purifying, absorbing and recycling chlorinated gas in benzene chlorination process |
| CN106000075B (en) * | 2016-07-08 | 2018-10-26 | 浙江闰土新材料有限公司 | The purification absorption of chlorinated exhaust and circulation utilization method and device in benzene chloridization process |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080716 |