CN102557923A - Method for purifying benzoyl chloride reaction terminating solution - Google Patents
Method for purifying benzoyl chloride reaction terminating solution Download PDFInfo
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- CN102557923A CN102557923A CN2011103940782A CN201110394078A CN102557923A CN 102557923 A CN102557923 A CN 102557923A CN 2011103940782 A CN2011103940782 A CN 2011103940782A CN 201110394078 A CN201110394078 A CN 201110394078A CN 102557923 A CN102557923 A CN 102557923A
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- benzoyl chloride
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- chloride 99min
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Abstract
The invention discloses a method for purifying a benzoyl chloride reaction terminating solution. The method comprises the following steps of: reacting benzotrichloride serving as a main raw material with benzoic acid or water in the presence of a ferric trichloride catalyst to prepare a benzoyl chloride reaction terminating solution, performing precision filtration through active carbon in a metal filter at a certain temperature to obtain a benzoyl chloride finished product, regenerating the active carbon, and collecting a ferric trichloride solution and a benzoic acid solid for recycling. The method is simple in operation process, 'three wastes' are nearly not produced in the whole production process, the yield and the quality of the product are high, and the method is an ideal green environment-friendly process.
Description
Technical field
The present invention relates to the production technique of Benzoyl chloride 99min., particularly relate to the method for purification that a kind of Benzoyl chloride 99min. reaction finishes liquid, belong to organic chemistry adsorption separation technology field.
Background technology
Benzoyl chloride 99min., molecular formula are C
7H
5ClO, molecular weight are 140.57, and Chinese is a Benzoyl chloride 99min., benzoyl chloride, and benzoyl chloride, the water white transparency inflammable liquid is exposed in the air and promptly is fuming.Special pungent odour is arranged.Steam has tearing property.Zero pour-1.0 ℃, fusing point-1.0 ℃, 197.2 ℃ of boiling points, 71 ℃ (1.2kPa), specific density 1.2120 (20/4 ℃), specific refractory power 1.5537,88 ℃ of flash-points.Be dissolved in ether, chloroform, benzene and dithiocarbonic anhydride.Meet water, ammonia or ethanol and decompose gradually, generate phenylformic acid, BM or ethyl benzoate and hydrogenchloride.
Benzoyl chloride 99min. is made initiator BPO, peroxidized t-butyl perbenzoate, pesticide herbicide etc. as organic synthesis, dyestuff and medical material.Aspect agricultural chemicals, be novel induction type sterilant isoxzzole sulphur phosphorus midbody.Benzoyl chloride 99min. is important benzoylation and benzyl reagent.Most of Benzoyl chloride 99min. is used for producing Lucidol, and next is used to produce the important industrial chemicals of benzophenone, peruscabin, benzyl cellulose and BM etc.Lucidol is used for the polymerization starter of plastic monomer, the catalyzer that polyester, epoxy, vinyl resin are produced, the self-solidifying agent of glass fiber material, and the linking agent of fluosilicic rubber, grease is refining, bleaching of flour, fiber decolouring etc.
It is raw material that main employing trichlorotoluene zotrichloride and phenylformic acid or water are gone up in Benzoyl chloride 99min. industry at present, produces Benzoyl chloride 99min. with iron trichloride as catalyzer, and the Benzoyl chloride 99min. of generation is purified through the distillation tower distillation.But this method energy consumption is big, and yield is low, inconvenient operation; Because reaction finishes to have the catalyzer iron trichloride in the liquid, cause being difficult to steamed fully, and mutability is yellow easily simultaneously to the later stage Benzoyl chloride 99min.; Cause quality product to reduce, and produce a large amount of trade waste (the Benzoyl chloride 99min. still is residual), this refuse environmental pollution is very big; Be difficult for being processed, wherein also contain a large amount of iron trichlorides and a spot of phenylformic acid is not recycled.Cause the waste on the resource.Therefore, the post-treating method that Benzoyl chloride 99min. reaction in the prior art is finished liquid improves, and has huge economic benefit and social benefit, meets requirements of green environmental protection again.
Summary of the invention
The technical problem that the present invention mainly solves provides a kind of simple and easy to do, method of purification that Benzoyl chloride 99min. reaction that embody economy and clean production finishes liquid.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of reaction for preparing Benzoyl chloride 99min. finishes the method for purification of liquid, is main raw material and phenylformic acid or water carry out the prepared in reaction Benzoyl chloride 99min. at ferric chloride catalyst reaction end liquid with trichlorotoluene zotrichloride; At a certain temperature; Carry out secondary filter through the gac in the metallic filter, obtain the Benzoyl chloride 99min. finished product, again with regeneration of activated carbon; Collect liquor ferri trichloridi and solid phenylformic acid, recycle again.
In preferred embodiment of the present invention, described metallic filter is the acid resistance metal alloy compositions.
In preferred embodiment of the present invention, described metallic filter is the titanium alloy alloy material.
In preferred embodiment of the present invention, described gac is ball-type or column type gac, and the aperture is 10 μ m-100 μ m.
In preferred embodiment of the present invention, described gac is 1-3:100 with the mass ratio that reaction finishes night.
In preferred embodiment of the present invention, the aperture of the filter bag of described metallic filter is 1 μ m-50 μ m.
In preferred embodiment of the present invention, the aperture of the filter bag of described metallic filter is 4.5 μ m-5.0 μ m.
In preferred embodiment of the present invention, described temperature is 20-50 ℃.
Technical scheme provided by the invention adopts the gac in the metallic filter to carry out secondary filter; Get the Benzoyl chloride 99min. finished product, again with regeneration of activated carbon, isolated catalyzer iron trichloride and phenylformic acid utilize again; Operating procedure is simple; Produce hardly in the whole process of production " three wastes ", the yield of product and quality are high, are the ideal green environment-protective process.
Embodiment
A kind of reaction for preparing Benzoyl chloride 99min. finishes the method for purification of liquid; With trichlorotoluene zotrichloride is that main raw material and phenylformic acid or water finish liquid in the reaction that ferric chloride catalyst carries out the prepared in reaction Benzoyl chloride 99min., at a certain temperature, carries out secondary filter through the gac in the metallic filter; Get the Benzoyl chloride 99min. finished product; With regeneration of activated carbon, collect liquor ferri trichloridi and solid phenylformic acid again, recycle again.
Wherein, described metallic filter is the acid resistance metal alloy compositions, preferred titanium alloy alloy material; Described gac is ball-type or column type gac, and the aperture is 10 μ m-100 μ m; Described gac is 1-3:100 with the mass ratio that reaction finishes night; The aperture of the filter bag of described metallic filter is 1 μ m-50 μ m, and preferred aperture is 4.5 μ m-5.0 μ m; Described temperature is 20-50 ℃.
Execute example 1
Be that the ball shape active carbon of 50um is inserted and had in the strainer of titanium alloy of filter bag that the aperture is 1um earlier with the 1kg aperture; Then 100kg being cooled to 20 ℃ Benzoyl chloride 99min. reaction finishes liquid pump and goes into to be filled with having in the strainer of titanium alloy of filter bag that the aperture is 1um of ball shape active carbon; After the filtration; Get the finished product Benzoyl chloride 99min., content is 99.6%.With ball shape active carbon regeneration, collect liquor ferri trichloridi and solid phenylformic acid afterwards.
Embodiment 2
Be that the ball shape active carbon of 100um is inserted and had in the strainer of titanium alloy of filter bag that the aperture is 4.5um earlier with the 3kg aperture; Then 100kg being cooled to 50 ℃ Benzoyl chloride 99min. reaction finishes liquid pump and goes into to be filled with having in the strainer of titanium alloy of filter bag that the aperture is 4.5um of cylindricality gac; After the filtration; Get the finished product Benzoyl chloride 99min., content is 99.5%.With the cylindricality regeneration of activated carbon, collect liquor ferri trichloridi and solid phenylformic acid afterwards.
Embodiment 3
Be that the cylindricality gac of 10um is inserted and had in the strainer of titanium alloy of filter bag that the aperture is 5.0um earlier with the 2kg aperture; Then 100kg being cooled to 30 ℃ Benzoyl chloride 99min. reaction finishes liquid pump and goes into to be filled with having in the strainer of titanium alloy of filter bag that the aperture is 5.0um of cylindricality gac; After the filtration; Get the finished product Benzoyl chloride 99min., content is 99.7%.With the cylindricality regeneration of activated carbon, collect liquor ferri trichloridi and solid phenylformic acid afterwards.
Embodiment 4
Be that the ball shape active carbon of 50um is inserted and had in the strainer of titanium alloy of filter bag that the aperture is 5.0um earlier with the 2kg aperture; Then 100kg being cooled to 30 ℃ Benzoyl chloride 99min. reaction finishes liquid pump and goes into to be filled with having in the strainer of titanium alloy of filter bag that the aperture is 5.0um of cylindricality gac; After the filtration; Get the finished product Benzoyl chloride 99min., content is 99.9%.With the cylindricality regeneration of activated carbon, collect liquor ferri trichloridi and solid phenylformic acid afterwards.
Embodiment 5
Be that the cylindricality gac of 30um is inserted and had in the strainer of titanium alloy of filter bag that the aperture is 4.5um earlier with the 3kg aperture; Then 100kg being cooled to 30 ℃ Benzoyl chloride 99min. reaction finishes liquid pump and goes into to be filled with having in the strainer of titanium alloy of filter bag that the aperture is 4.5um of cylindricality gac; After the filtration; Get the finished product Benzoyl chloride 99min., content is 99.7%.With the cylindricality regeneration of activated carbon, collect liquor ferri trichloridi and solid phenylformic acid afterwards.
The above is merely embodiments of the invention; Be not so limit claim of the present invention; Every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; Or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (8)
1. a reaction for preparing Benzoyl chloride 99min. finishes the method for purification of liquid, it is characterized in that, and be main raw material and phenylformic acid or water carry out the prepared in reaction Benzoyl chloride 99min. at ferric chloride catalyst reaction end liquid with trichlorotoluene zotrichloride; At a certain temperature; Carry out secondary filter through the gac in the metallic filter, get the Benzoyl chloride 99min. finished product, again with regeneration of activated carbon; Collect liquor ferri trichloridi and solid phenylformic acid, recycle again.
2. the reaction of Benzoyl chloride 99min. according to claim 1 finishes the method for purification of liquid, it is characterized in that described metallic filter is the acid resistance metal alloy compositions.
3. the reaction of Benzoyl chloride 99min. according to claim 2 finishes the method for purification of liquid, it is characterized in that described metallic filter is the titanium alloy alloy material.
4. the reaction of Benzoyl chloride 99min. according to claim 1 finishes the method for purification of liquid, it is characterized in that described gac is ball-type or column type gac, and the aperture is 10 μ m-100 μ m.
5. the reaction of Benzoyl chloride 99min. according to claim 1 finishes the method for purification of liquid, it is characterized in that, described gac is 1-3:100 with the mass ratio that reaction finishes night.
6. the reaction of Benzoyl chloride 99min. according to claim 1 finishes the method for purification of liquid, it is characterized in that the aperture of the filter bag of described metallic filter is 1 μ m-50 μ m.
7. the reaction of Benzoyl chloride 99min. according to claim 6 finishes the method for purification of liquid, it is characterized in that the aperture of the filter bag of described metallic filter is 4.5 μ m-5.0 μ m.
8. the reaction of Benzoyl chloride 99min. according to claim 1 finishes the method for purification of liquid, it is characterized in that described temperature is 20-50 ℃.
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| CN2011103940782A CN102557923A (en) | 2011-12-02 | 2011-12-02 | Method for purifying benzoyl chloride reaction terminating solution |
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| CN2011103940782A CN102557923A (en) | 2011-12-02 | 2011-12-02 | Method for purifying benzoyl chloride reaction terminating solution |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175242A (en) * | 2015-09-14 | 2015-12-23 | 宜都市友源实业有限公司 | Method for recycling trichlorotoluene and/or benzoyl chloride waste slag |
| CN105384625A (en) * | 2015-12-17 | 2016-03-09 | 湖北相和精密化学有限公司 | 3-chloro methyl benzoyl chloride synthetic method |
Citations (6)
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| US4276231A (en) * | 1978-09-23 | 1981-06-30 | Bayer Aktiengesellschaft | Process for the preparation of optionally substituted benzoyl chloride |
| CN1148588A (en) * | 1996-05-17 | 1997-04-30 | 常熟市金城化工厂 | Method for recovering residues in benzoyl chloride distillation pot |
| JPH11171825A (en) * | 1997-12-05 | 1999-06-29 | Nippon Light Metal Co Ltd | Production of benzoyl chloride |
| CN1508115A (en) * | 2002-12-13 | 2004-06-30 | 上海群力化工有限公司 | High-purity benzoyl chloride synthesizing process |
| CN101601989A (en) * | 2009-06-29 | 2009-12-16 | 云南大学 | The method of a kind of liquid absorbent and improvement water body in lake arsenic contamination |
| CN101934221A (en) * | 2010-10-14 | 2011-01-05 | 厦门大学 | Modified adsorbent and preparation method thereof |
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2011
- 2011-12-02 CN CN2011103940782A patent/CN102557923A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4276231A (en) * | 1978-09-23 | 1981-06-30 | Bayer Aktiengesellschaft | Process for the preparation of optionally substituted benzoyl chloride |
| CN1148588A (en) * | 1996-05-17 | 1997-04-30 | 常熟市金城化工厂 | Method for recovering residues in benzoyl chloride distillation pot |
| JPH11171825A (en) * | 1997-12-05 | 1999-06-29 | Nippon Light Metal Co Ltd | Production of benzoyl chloride |
| CN1508115A (en) * | 2002-12-13 | 2004-06-30 | 上海群力化工有限公司 | High-purity benzoyl chloride synthesizing process |
| CN101601989A (en) * | 2009-06-29 | 2009-12-16 | 云南大学 | The method of a kind of liquid absorbent and improvement water body in lake arsenic contamination |
| CN101934221A (en) * | 2010-10-14 | 2011-01-05 | 厦门大学 | Modified adsorbent and preparation method thereof |
Non-Patent Citations (1)
| Title |
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| V.FIERRO等: "Arsenic removal by iron-doped activated carbons prepared by ferric chloride forced hydrolysis", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175242A (en) * | 2015-09-14 | 2015-12-23 | 宜都市友源实业有限公司 | Method for recycling trichlorotoluene and/or benzoyl chloride waste slag |
| CN105384625A (en) * | 2015-12-17 | 2016-03-09 | 湖北相和精密化学有限公司 | 3-chloro methyl benzoyl chloride synthetic method |
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Application publication date: 20120711 |