CN104086352A - Method for synthesizing m-dichlorobenzene from m-dinitrobenzene - Google Patents
Method for synthesizing m-dichlorobenzene from m-dinitrobenzene Download PDFInfo
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- CN104086352A CN104086352A CN201410268254.1A CN201410268254A CN104086352A CN 104086352 A CN104086352 A CN 104086352A CN 201410268254 A CN201410268254 A CN 201410268254A CN 104086352 A CN104086352 A CN 104086352A
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- dichlorobenzene
- meta
- dinitrobenzene
- chlorination reaction
- reaction still
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Abstract
A method for synthesizing m-dichlorobenzene from m-dinitrobenzene relates to the technical filed of the chemical industry. The method comprises the following steps: mixing m-dinitrobenzene with a catalyst, melting the obtained mixture, adding the molten mixture into a chlorination reaction kettle, heating to 210-230DEG C, introducing chlorine into the reaction kettle under a flow of 10kg/h, continuously adding m-dinitrobenzene after material condensation under a flow of 15kg/h, collecting the chlorinated condensate liquid in the reaction kettle, adding weak aqua ammonia to neutralize in order to adjust the pH value to 7, adding water, and washing to obtain crude m-dichlorobenzene; and heating to make the temperature in the kettle reach 100DEG C, carrying out reduced pressure distillation on the crude m-dichlorobenzene to obtain finished m-dichlorobenzene, packaging, and warehousing. The method has the advantages of convenient and simple preparation, small amount of generated waste acids, easily available materials, less equipment investment, high purity, convenient operation and low production cost, and the prepared m-dichlorobenzene has the advantages of good use effect, safety and reliability.
Description
Technical field
The present invention relates to chemical technology field, be specifically related to the method by the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene.
Background technology
Meta Dichlorobenzene is colourless liquid, irritant smell.Water insoluble, be dissolved in alcohol, ether.Can carry out chlorination, nitrated, sulfonation, hydrolysis reaction, meet reactive aluminum violent, for organic synthesis.Meta Dichlorobenzene through reacting, obtains 2,4 with chloroacetyl chloride, and-Trichloroacetophenon, as the intermediate of broad-spectrum antifungal medicine miconazole.Under the condition that has iron(ic) chloride or aluminium mercury, carry out chlorination reaction, mainly generate 1,2,4-trichlorobenzene.Exist under the condition of catalyzer, in 550-850 ℃ of hydrolysis, generate m-Chlorophenol and Resorcinol.Take cupric oxide as catalyzer, depress 150-200 ℃ and react with strong aqua and generate mphenylenediamine adding.The production technique of preparing Resorcinol on chemical engineering industry is comparatively complicated, and the purity of producing is lower, is difficult to meet the demand of human being's production life.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method simple, the method by the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene of energy-conserving and environment-protective.
Technical problem to be solved by this invention realizes by the following technical solutions:
Method by the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene, is characterized in that: comprise following processing step,
A. then Meta-dinitrobenzene and catalyst mix melted and then dropped in chlorination reaction still.
While b. the temperature in chlorination reaction still being risen to 210-230 ℃, chlorine is passed in chlorination reaction still, the flow control of chlorine input is at 10kg/h.
C. after there is material condensation, continue to add Meta-dinitrobenzene, the flow control adding is at 15kg/h.
D. by the condensed fluid collection after chlorination in reactor.
E. then the phlegma of collecting in d is added weak ammonia to be neutralized to PH=7 and then add water washing.
F. the mixture after washing is carried out to separation and obtain thick Meta Dichlorobenzene.
G. temperature in the kettle being risen to 100 ℃ then carries out thick Meta Dichlorobenzene underpressure distillation and obtains Meta Dichlorobenzene finished product packing warehouse-in.
The waste water producing in mixture in described step f after separation directly enters wastewater disposal basin and in wastewater disposal basin, adds weak ammonia.
The catalyzer using in described step a is cupric oxide.
The invention has the beneficial effects as follows: the present invention is easy to prepare simple, and spent acid generation is few, and raw material is easy to get, and facility investment is few, and purity is high, convenient operation, production cost is low, and the Meta Dichlorobenzene result of use of preparation is good, safe and reliable.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach object and effect is easy to understand, below in conjunction with specific embodiment, further set forth the present invention.
Method by the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene, is characterized in that: comprise following processing step,
B. Meta-dinitrobenzene is mixed to then fusing then drop in chlorination reaction still with copper oxide catalyst.
While b. the temperature in chlorination reaction still being risen to 210-230 ℃, chlorine is passed in chlorination reaction still, the flow control of chlorine input is at 10kg/h.
C. after there is material condensation, continue to add Meta-dinitrobenzene, the flow control adding is at 15kg/h.
D. by the condensed fluid collection after chlorination in reactor.
E. then the phlegma of collecting in d is added weak ammonia to be neutralized to PH=7 and then add water washing.
F. the mixture after washing is carried out to separation and obtain thick Meta Dichlorobenzene, the waste water producing in the mixture after separation directly enters wastewater disposal basin and in wastewater disposal basin, adds weak ammonia.
G. temperature in the kettle being risen to 100 ℃ then carries out thick Meta Dichlorobenzene underpressure distillation and obtains Meta Dichlorobenzene finished product packing warehouse-in.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (3)
1. by the method for the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene, it is characterized in that: comprise following processing step,
A. then Meta-dinitrobenzene and catalyst mix melted and then dropped in chlorination reaction still.
While b. the temperature in chlorination reaction still being risen to 210-230 ℃, chlorine is passed in chlorination reaction still, the flow control of chlorine input is at 10kg/h.
C. after there is material condensation, continue to add Meta-dinitrobenzene, the flow control adding is at 15kg/h.
D. by the condensed fluid collection after chlorination in reactor.
E. then the phlegma of collecting in d is added weak ammonia to be neutralized to PH=7 and then add water washing.
F. the mixture after washing is carried out to separation and obtain thick Meta Dichlorobenzene.
G. temperature in the kettle being risen to 100 ℃ then carries out thick Meta Dichlorobenzene underpressure distillation and obtains Meta Dichlorobenzene finished product packing warehouse-in.
2. the method by the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene according to claim 1, is characterized in that: the waste water producing in the mixture in described step f after separation directly enters wastewater disposal basin and in wastewater disposal basin, adds weak ammonia.
3. the method by the synthetic Meta Dichlorobenzene of Meta-dinitrobenzene according to claim 1, is characterized in that: the catalyzer using in described step a is cupric oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410268254.1A CN104086352A (en) | 2014-06-16 | 2014-06-16 | Method for synthesizing m-dichlorobenzene from m-dinitrobenzene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410268254.1A CN104086352A (en) | 2014-06-16 | 2014-06-16 | Method for synthesizing m-dichlorobenzene from m-dinitrobenzene |
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| CN104086352A true CN104086352A (en) | 2014-10-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410268254.1A Pending CN104086352A (en) | 2014-06-16 | 2014-06-16 | Method for synthesizing m-dichlorobenzene from m-dinitrobenzene |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365953A (en) * | 2016-08-29 | 2017-02-01 | 枣阳市众成化工有限公司 | M-dichlorobenzene production method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3917723A (en) * | 1972-11-16 | 1975-11-04 | Hoechst Ag | Process for the continuous manufacture of m-chloronitrobenzene from m-dinitrobenzene |
| US4952719A (en) * | 1984-10-15 | 1990-08-28 | Occidental Chemical Corporation | Process for the preparation of halo aromatic compounds |
| CN101085713A (en) * | 2007-06-29 | 2007-12-12 | 沈志良 | Method for synthesizing p-dichlorobenzene |
| CN101774885A (en) * | 2010-01-06 | 2010-07-14 | 安徽安生生物化工科技有限责任公司 | Method for synthesizing m-dichlorobenzene |
-
2014
- 2014-06-16 CN CN201410268254.1A patent/CN104086352A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3917723A (en) * | 1972-11-16 | 1975-11-04 | Hoechst Ag | Process for the continuous manufacture of m-chloronitrobenzene from m-dinitrobenzene |
| US4952719A (en) * | 1984-10-15 | 1990-08-28 | Occidental Chemical Corporation | Process for the preparation of halo aromatic compounds |
| CN101085713A (en) * | 2007-06-29 | 2007-12-12 | 沈志良 | Method for synthesizing p-dichlorobenzene |
| CN101774885A (en) * | 2010-01-06 | 2010-07-14 | 安徽安生生物化工科技有限责任公司 | Method for synthesizing m-dichlorobenzene |
Non-Patent Citations (1)
| Title |
|---|
| 张宝文: "由间二硝基苯合成间二氯苯", 《辽宁华工》, no. 2, 31 December 1996 (1996-12-31), pages 35 - 36 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365953A (en) * | 2016-08-29 | 2017-02-01 | 枣阳市众成化工有限公司 | M-dichlorobenzene production method |
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