CN101906043B - Production process for purifying high-purity 2,5-dichloronitrobenzene by solvent washing method - Google Patents
Production process for purifying high-purity 2,5-dichloronitrobenzene by solvent washing method Download PDFInfo
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- CN101906043B CN101906043B CN 201010256525 CN201010256525A CN101906043B CN 101906043 B CN101906043 B CN 101906043B CN 201010256525 CN201010256525 CN 201010256525 CN 201010256525 A CN201010256525 A CN 201010256525A CN 101906043 B CN101906043 B CN 101906043B
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Abstract
The invention mainly discloses a production process for purifying high-purity 2,5-dichloronitrobenzene by a solvent washing method, which is characterized by comprising the following steps: putting 2,5-dichloronitrobenzene containing 3,4-dichloronitrobenzene evenly in a centrifuge; adding hot water of 65 DEG C to the centrifuge for quickly melting the 3,4-dichloronitrobenzene in the mixture; centrifuging; and separating crystals from the mother solution to obtain the 2,5-dichloronitrobenzene of which the content is over 99.5%. The invention has the advantages of furthest improving the economic benefit by refining and processing a small batch of 2,5-dichloronitrobenzene by the method, reducing the environmental pollution and improving the sanitation and safety of an operational field.
Description
Technical field
It is a kind of 2 that the present invention relates generally to, and the production technique that the 5-dichloronitrobenzene is purified specifically adopts the solvent wash method to purify, and reaches can produce content at 2 more than 99.5%, the 5-dichloronitrobenzene.
Background technology
2,5-dichloronitrobenzene is a kind of important Organic Chemicals, as a kind of efficient people's nitrogen fertilizer potentiating agent and agricultural chemicals, medicine, the synthetic intermediate of dyestuff.
The santochlor that utilizes solid waste chlorobenzene coke tar to extract is raw material, extends the nitrogen fertilizer potentiating agent 2 of producing, the 5-dichloronitrobenzene; have the fixed nitrogen function of fertilizer retention, can prevent that soil moisture runs off, and improves the output of the farm crop such as paddy rice; be conducive to improve soil, preserve the ecological environment, realize low-carbon economy.
Use for guaranteeing safety and quality product, require the purity of 2,5-dichloronitrobenzene must be higher than 99.5%, and the santochlor that utilizes solid waste chlorobenzene tar to extract is raw material, extends and produces 2, and the 5-dichloronitrobenzene is because containing 3, the 4-dichloronitrobenzene, purity can not be up to standard.Because the content of raw material santochlor is lower, make 2 of generate subsequent output, 5-dichloronitrobenzene content only maintains between 97%～98%, guarantee 2,5-dichloronitrobenzene result of use is best, just must utilize a kind of method to content between 97%～98% 2, the 5-dichloronitrobenzene carries out separating-purifying, and does not find at present corresponding known technology.
Summary of the invention
Main task of the present invention is to provide a kind of 2, the production technique that the 5-dichloronitrobenzene is purified, specifically go out to contain 3 for the santochlor that utilizes solid waste chlorobenzene tar to extract for raw material production, 2 of 4-dichloronitrobenzene, 5-dichloronitrobenzene purity can not be up to standard, and the product content that can make of setting reaches 2 more than 99.5%, the production technique that the 5-dichloronitrobenzene is purified.
In order to solve above technical problem, the production technique of a kind of purifying high-purity 2,5-dichloronitrobenzeneby by solvent washing method of the present invention, it is characterized in that: will contain 3,2 of 4-dichloronitrobenzene, 5-dichloronitrobenzene evenly are preset in whizzer, import the hot water of 65 ℃ in whizzer, make 3 in mixture, the 4-dichloronitrobenzene melts as early as possible, and centrifugal treating, and crystal separates with mother liquor, obtain content at 2 more than 99.5%, the 5-dichloronitrobenzene.
Further, the hot water of described 65 ℃ with contain 2 of 3,4-dichloronitrobenzene, the mass ratio of 5-dichloronitrobenzene is 1: 5.
The invention has the advantages that:
It is simple that solvent wash method separation and purification 2,5-dichloronitrobenzene have equipment, invests littlely, and energy consumption is low, and processing condition are gentle, characteristics easy and simple to handle.Utilize 65 ℃ hot water to 97%～98% 2,5-dichloro nitro and 2%～3% 3, the mixture of 4-dichloronitrobenzene tentatively melts, and utilize whizzer to carry out solid-liquid separation to mixture, the purity of 2,5-dichloronitrobenzene can be brought up to more than 99.5%, yield is more than 90%, centrifuge mother liquor (water, 2,5-dichloronitrobenzene, 3, the mixing solutions of 4-dichloronitrobenzene) can further extract separation.Utilize present method refinement treatment short run 2, the 5-dichloronitrobenzene can be increased economic efficiency to greatest extent, reduces environmental pollution, improves operation place hygienic safety.
Embodiment
The present invention be directed to the santochlor that utilizes solid waste chlorobenzene coke tar to extract and be raw material, produce and contain 2 of 3,4-dichloronitrobenzene, the purifying technique that the 5--dichloronitrobenzene is made.
Because the content of raw material santochlor is lower, make 2 of generate subsequent output, 5-dichloronitrobenzene content only maintains between 97%～98%, guarantee 2,5-dichloronitrobenzene result of use is best, just must utilize a kind of method to content between 97%～98% 2, the 5-dichloronitrobenzene carries out separating-purifying.
Utilize gas chromatograph to this low levels 2, the 5-dichloronitrobenzene detects, its isomers 3, the 4-dichloronitrobenzene accounts for 2%～3%, according to 2,5-dichloronitrobenzene, 3, the difference (2 of 4-dichloronitrobenzene on fusing point, 56 ℃ of 5-dichloronitrobenzenes, 43 ℃ of 3,4-dichloronitrobenzenes), its physical property has obvious difference, therefore, selection will just can solve above technical problem in solvent between the two.
Below contrast and the analysis that concrete solvent is selected:
Physical property according to the product dichloronitrobenzene: 2,56 ℃ of 5-dichloronitrobenzene fusing points, 3,43 ℃ of 4-dichloronitrobenzene fusing points, it is dissolved in cold water hardly and is dissolved in various organic solvents, in conjunction with the principle of solvent wash method separating-purifying and the feasibility requirement of systemic circulation operation, washing composition should satisfy following primary condition:
(1) this solvent is to 2,5-dichloronitrobenzene, 3, and the solubleness of 4-dichloronitrobenzene is little;
(2) when this solvent has certain temperature, can improve preferably and be wrapped on a small quantity 3 in 2,5-dichloronitrobenzene, the fusing speed of 4-dichloronitrobenzene;
(3) can utilize centrifuging to process through 2 of washing, the 5-dichloronitrobenzene makes 3 of melting, 4-dichloronitrobenzene detachment system;
(4) can effectively separate centrifuge mother liquor;
(5) the washing composition cost is low, can realize batch production.
requirement accordingly, select temperature a little more than 2, 5-dichloronitrobenzene and 3, the high-temperature water of 4-dichloronitrobenzene fusing point is as washing composition, contrast 2 by lab scale, 5-dichloronitrobenzene and 3, the fusing speed of the mixture of 4-dichloronitrobenzene in the aqueous solution of 58 ℃～65 ℃, discovery is in the aqueous solution of 58 ℃, 3, the melting of 4-dichloronitrobenzene is very slow, along with the hot water temperature is elevated to 65 ℃ gradually, when 2, 5-dichloronitrobenzene generating unit is divided when melting, 3, the fusing speed of 4-dichloronitrobenzene is the fastest, when continuing rising temperature to 70 ℃, 3, the fusing speed of 4-dichloronitrobenzene does not advance obvious quickening, cause on the contrary 2, the 5-dichloronitrobenzene produces fuzzy shape.As seen the hot water of 65 ℃ is to make preferably to be entrained in 2, in the 5-dichloronitrobenzene 3, the 4-dichloronitrobenzene accelerates the solvent of melting, and not only the melting selectivity to 3,4-dichloronitrobenzene is high for it, to target product 2, the solubleness of 5-dichloronitrobenzene is very little, and 3,4-dichloronitrobenzene is water insoluble, these characteristics both had been conducive to improve separating effect, were conducive to again the subsequent purification centrifuge mother liquor.
Draw according to above-mentioned test, it is the hot water of 65 ℃ that solvent is quoted temperature.
After having chosen solvent, by purifying, concrete steps are as follows:
The santochlor that utilizes solid waste chlorobenzene coke tar to extract is raw material, produce 97%～98% 2, the 5-dichloronitrobenzene and 2%～3% 3, the mixture of 4-dichloronitrobenzene evenly is preset in whizzer, import the hot water of 65 ℃ in whizzer, make 3 in mixture, the 4-dichloronitrobenzene melts ,-as the patent ratio of hot water and mixture be 1: 5; Process centrifugal treating 15 minutes, crystal separates with mother liquor, just can obtain content at 2 more than 99.5%, the 5-dichloronitrobenzene.
Whole solvent extraction purification separating high-purity 2, the 5-dichloronitrobenzene is the intermittent type batch operation, the concrete adjustment using amount of hot water and the centrifugation time that according to gas chromatograph, the content of finished product detection are just come by operator, until finished product 2,5-dichloronitrobenzene content is higher than till 99.5%.
Claims (1)
1. solvent wash method purification high purity 2, the production technique of 5-dichloronitrobenzene is characterized in that: with 97%～98% 2, the 5-dichloronitrobenzene and 2%～3% 3, the mixture of 4-dichloronitrobenzene evenly is preset in whizzer, import the hot water of 65 ℃ in whizzer, make 3 in mixture, the 4-dichloronitrobenzene melts as early as possible, and centrifugal treating, crystal separates with mother liquor, obtains content at 2 more than 99.5%, the 5-dichloronitrobenzene; The hot water of described 65 ℃ with contain 2 of 3,4-dichloronitrobenzene, the mass ratio of 5-dichloronitrobenzene is 1: 5.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010256525 CN101906043B (en) | 2010-08-19 | 2010-08-19 | Production process for purifying high-purity 2,5-dichloronitrobenzene by solvent washing method |
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| CN 201010256525 CN101906043B (en) | 2010-08-19 | 2010-08-19 | Production process for purifying high-purity 2,5-dichloronitrobenzene by solvent washing method |
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| CN101906043A CN101906043A (en) | 2010-12-08 |
| CN101906043B true CN101906043B (en) | 2013-06-12 |
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| CN109535002B (en) * | 2019-01-25 | 2023-09-26 | 中触媒新材料股份有限公司 | Method for separating 2, 3-dichloronitrobenzene from dichloronitrobenzene isomer by crystallization |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1322020A (en) * | 1969-11-21 | 1973-07-04 | Hoechst Ag | Process for the separation of isomer mixtures |
| CN1117038A (en) * | 1994-12-29 | 1996-02-21 | 浙江大学 | Synthetic process of 2,4-fluobenzene dichloride |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1322020A (en) * | 1969-11-21 | 1973-07-04 | Hoechst Ag | Process for the separation of isomer mixtures |
| CN1117038A (en) * | 1994-12-29 | 1996-02-21 | 浙江大学 | Synthetic process of 2,4-fluobenzene dichloride |
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