CN102675039A - Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials - Google Patents
Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials Download PDFInfo
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- CN102675039A CN102675039A CN2012101885323A CN201210188532A CN102675039A CN 102675039 A CN102675039 A CN 102675039A CN 2012101885323 A CN2012101885323 A CN 2012101885323A CN 201210188532 A CN201210188532 A CN 201210188532A CN 102675039 A CN102675039 A CN 102675039A
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- santochlor
- dichlorobenzene
- transposition
- technology
- paradichlorobenzene
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Abstract
The invention discloses a process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials. The process mainly comprises the following steps of: rectifying the chloridized aromatic hydrocarbon waste to obtain high-concentration paradichlorobenzene; preparing high-content paradichlorobenzene by a crystallization technology by using a paradichlorobenzene solution; inverting the high-content paradichlorobenzene into low-concentration paradichlorobenzene by a normal pressure inversion technology; washing with water; and crystallizing and purifying. According to the process, the chloridized aromatic hydrocarbon waste is used as the raw materials, the high-content paradichlorobenzene is separated by a separation technology, the high-concentration paradichlorobenzene is prepared by normal-pressure acylation reaction, and the high-content m-dichlorobenzene is extracted by the crystallization technology.
Description
Technical field
The present invention relates to a kind of production technique of Meta Dichlorobenzene.
Background technology
The use of Meta Dichlorobenzene is very wide on the industrial production, but producing of Meta Dichlorobenzene is comparatively difficult, so the price of Meta Dichlorobenzene is higher relatively, and how producing high-load Meta Dichlorobenzene becomes an important topic.
Chlorobenzene carries out being prone to form the chlorinated aromatics waste behind the oriented chlorination; Wherein the overwhelming majority is santochlor and orthodichlorobenzene; The Meta Dichlorobenzene that only contains minute quantity; Therefore working out a kind of safe and reliable chlorinated aromatics waste that utilizes is one of a lot of colleges and universities and institute difficult point of capturing at present for the process method of raw material production Meta Dichlorobenzene, does not see relevant report so far.
Summary of the invention
Main task of the present invention is to provide a kind of production technique of Meta Dichlorobenzene, specifically is a kind ofly from waste, to extract, and effectively utilizes the production technique of waste and protection environment.
In order to solve above technical problem, of the present invention a kind of be the technology of raw material production Meta Dichlorobenzene with the chlorinated aromatics waste, be mainly the chlorinated aromatics waste through rectification process, obtain the santochlor of higher concentration; This santochlor solution is made the high-content santochlor through crystallization technique; It is characterized in that: said step also comprises: utilize the santochlor of normal pressure transposition technology with high-content santochlor transposition low concentration; Step is following: in the transposition still, add santochlor, logical steam heats up while feeding in raw material, and controls 60-70 ℃ of still temperature, after treating to dissolve fully, adds aluminum chloride, drips water, strengthens quantity of steam, is warmed up to 170 ℃ rapidly, is incubated 3 hours down at 170 ℃.
Washing after the transposition: transposition is cooled to below 100 ℃ after finishing, and adds entry, leaves standstill after the stirring about 1 hour, and significantly layering of back, the upper strata is an aluminum chloride acid waste water, lower floor is a mixed dichlorobenzene.
Crystallization and purification: will wash isolated mixed dichlorobenzene and deliver to mold, crystallization goes out santochlor, the Meta Dichlorobenzene of purifying out.
Further, said santochlor: aluminum chloride: the mass ratio of water is=200:10:1.
Advantage of the present invention: utilize the chlorinated aromatics waste to be raw material, tell the high-content santochlor, make the Meta Dichlorobenzene of higher concentration again through the normal pressure acylation reaction, extract high-load Meta Dichlorobenzene again through crystallization technique at last through stripping technique.
Embodiment
Embodiment 1
Technology of the present invention is following:
1,, obtains the santochlor of higher concentration with chlorinated aromatics waste process rectification process; (routine)
2, this santochlor solution is made the high-content santochlor through crystallization technique; (routine)
3, utilize the santochlor of normal pressure transposition technology with high-content santochlor transposition low concentration;
3.1 detailed process is following: in the transposition still, add the 800kg santochlor, logical steam heats up while feeding in raw material, 60-70 ℃ of control still temperature; After treating to dissolve fully, add 40kg water aluminum chloride, drip 4kg water; Strengthen quantity of steam, be warmed up to 170 ℃ rapidly, be incubated 3 hours down at 170 ℃.
3.2 the washing after the transposition
Transposition is cooled to below 100 ℃ after finishing, and adds 200kg water, leave standstill after the stirring about 1 hour, and significantly layering of back, the upper strata is an aluminum chloride acid waste water, lower floor is a mixed dichlorobenzene.
4, crystallization and purification
To wash isolated mixed dichlorobenzene and deliver to mold, crystallization goes out santochlor, the Meta Dichlorobenzene of purifying out, and two cl contenies are more than 95% between assurance.
Claims (2)
1. one kind is the technology of raw material production Meta Dichlorobenzene with the chlorinated aromatics waste, is mainly chlorinated aromatics waste process rectification process, obtains the santochlor of higher concentration; This santochlor solution is made the high-content santochlor through crystallization technique; It is characterized in that: said step also comprises: utilize the santochlor of normal pressure transposition technology with high-content santochlor transposition low concentration; Step is following: in the transposition still, add santochlor, logical steam heats up while feeding in raw material, and controls 60-70 ℃ of still temperature, after treating to dissolve fully, adds aluminum chloride, drips water, strengthens quantity of steam, is warmed up to 170 ℃ rapidly, is incubated 3 hours down at 170 ℃; Washing after the transposition: transposition is cooled to below 100 ℃ after finishing, and adds entry, leaves standstill after the stirring about 1 hour, and significantly layering of back, the upper strata is an aluminum chloride acid waste water, lower floor is a mixed dichlorobenzene; Crystallization and purification: will wash isolated mixed dichlorobenzene and deliver to mold, crystallization goes out santochlor, the Meta Dichlorobenzene of purifying out.
2. according to claim 1 a kind of be the technology of raw material production Meta Dichlorobenzene with the chlorinated aromatics waste, said santochlor: aluminum chloride: the mass ratio of water is=200:10:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101885323A CN102675039A (en) | 2012-06-11 | 2012-06-11 | Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101885323A CN102675039A (en) | 2012-06-11 | 2012-06-11 | Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials |
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| Publication Number | Publication Date |
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| CN102675039A true CN102675039A (en) | 2012-09-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012101885323A Pending CN102675039A (en) | 2012-06-11 | 2012-06-11 | Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708994A (en) * | 2014-01-15 | 2014-04-09 | 黑龙江大学 | Method for preparing m-dichlorobenzene through catalysis of nano ZSM-5 molecular sieve and isomerization of p-dichlorobenzene |
| CN105037082A (en) * | 2015-06-10 | 2015-11-11 | 张家港市新盛新材料有限公司 | Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor |
| WO2016008175A1 (en) * | 2014-07-18 | 2016-01-21 | 江苏隆昌化工有限公司 | Method for separating and purifying p-dichlorobenzene |
| CN110922322A (en) * | 2019-11-01 | 2020-03-27 | 江苏隆昌化工有限公司 | Clean production method for improving reaction yield of 2, 4-dichloroacetophenone |
| CN111484390A (en) * | 2020-03-24 | 2020-08-04 | 江苏淮江科技有限公司 | Process for preparing m-dichlorobenzene by transposition of o-dichlorobenzene |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2819321A (en) * | 1955-05-23 | 1958-01-07 | Columbia Southern Chem Corp | Dichlorobenzene manufacture |
| CN101580456A (en) * | 2009-04-27 | 2009-11-18 | 江苏隆昌化工有限公司 | Kettle type crystallization process of paradichlorobenzene in solid waste benzene chloride tar |
| CN101696151A (en) * | 2009-10-12 | 2010-04-21 | 江苏依柯化工有限公司 | Synthetic method of m-dichlorobenzene |
| CN102358718A (en) * | 2011-09-05 | 2012-02-22 | 江苏隆昌化工有限公司 | Method for producing o-nitro-p-chloroaniline by using chloridized aromatic hydrocarbon waste as raw material |
-
2012
- 2012-06-11 CN CN2012101885323A patent/CN102675039A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2819321A (en) * | 1955-05-23 | 1958-01-07 | Columbia Southern Chem Corp | Dichlorobenzene manufacture |
| CN101580456A (en) * | 2009-04-27 | 2009-11-18 | 江苏隆昌化工有限公司 | Kettle type crystallization process of paradichlorobenzene in solid waste benzene chloride tar |
| CN101696151A (en) * | 2009-10-12 | 2010-04-21 | 江苏依柯化工有限公司 | Synthetic method of m-dichlorobenzene |
| CN102358718A (en) * | 2011-09-05 | 2012-02-22 | 江苏隆昌化工有限公司 | Method for producing o-nitro-p-chloroaniline by using chloridized aromatic hydrocarbon waste as raw material |
Non-Patent Citations (1)
| Title |
|---|
| 庞琰玲等: "常压转位制间二氯苯的试验研究", 《化工科技》, vol. 8, no. 05, 30 October 2000 (2000-10-30), pages 17 - 18 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103708994A (en) * | 2014-01-15 | 2014-04-09 | 黑龙江大学 | Method for preparing m-dichlorobenzene through catalysis of nano ZSM-5 molecular sieve and isomerization of p-dichlorobenzene |
| CN103708994B (en) * | 2014-01-15 | 2016-09-21 | 黑龙江大学 | The method that nano-ZSM-5 molecular sieve catalysis paracide isomerization prepares m-dichlorobenzene |
| WO2016008175A1 (en) * | 2014-07-18 | 2016-01-21 | 江苏隆昌化工有限公司 | Method for separating and purifying p-dichlorobenzene |
| CN105037082A (en) * | 2015-06-10 | 2015-11-11 | 张家港市新盛新材料有限公司 | Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor |
| CN110922322A (en) * | 2019-11-01 | 2020-03-27 | 江苏隆昌化工有限公司 | Clean production method for improving reaction yield of 2, 4-dichloroacetophenone |
| CN111484390A (en) * | 2020-03-24 | 2020-08-04 | 江苏淮江科技有限公司 | Process for preparing m-dichlorobenzene by transposition of o-dichlorobenzene |
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Application publication date: 20120919 |