CN106008223B - A kind of method of nitrofying aromatic hydrocarbon chloride - Google Patents
A kind of method of nitrofying aromatic hydrocarbon chloride Download PDFInfo
- Publication number
- CN106008223B CN106008223B CN201610371878.5A CN201610371878A CN106008223B CN 106008223 B CN106008223 B CN 106008223B CN 201610371878 A CN201610371878 A CN 201610371878A CN 106008223 B CN106008223 B CN 106008223B
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- Prior art keywords
- aromatic hydrocarbon
- hydrocarbon chloride
- solid
- nitrofying
- solid acid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
Abstract
The present invention relates to a kind of methods of nitrofying aromatic hydrocarbon chloride, aromatic hydrocarbon chloride and solid acid catalyst are put into reaction vessel, then be added anhydrous cupric sulfate or other similar to sulfate, be stirred continuously, after stirring evenly, fuming nitric aicd is slowly added dropwise again, then 1~5 hour is kept the temperature at 55~75 DEG C, after heat preservation, is separated by solid-liquid separation, solid after separation melts down drying, recycles；Liquid is washed with hot water, and then spontaneous nucleation obtains product.The advantage of the invention is that：The method of nitrofying aromatic hydrocarbon chloride of the present invention, by selecting suitable solid acid catalyst to carry out nitration reaction so that product purity and conversion ratio are further promoted, and solid acid can recycle, and do not generate waste, the theory of composite green environmental protection substantially.
Description
Technical field
The invention belongs to chemical technology field, more particularly to a kind of method of nitrofying aromatic hydrocarbon chloride.
Background technology
Aromatic hydrocarbon chloride is generally required by nitration reaction, is prepared into product containing aromatic hydrocarbon chloride.Traditional nitration reaction
In, generally using liquid mixed acid as catalyst progress nitration reaction after the completion of nitrification, a large amount of spent acid is will produce, can not be located
Reason, thus can welding.
Therefore, a kind of method for researching and developing no waste generation and environmentally protective nitrofying aromatic hydrocarbon chloride is to be highly desirable
's.
Invention content
The technical problem to be solved in the present invention is to provide a kind of no waste generation and environmentally protective nitrofying aromatic hydrocarbon chlorinations
The method of object.
In order to solve the above technical problems, the technical scheme is that：A kind of method of nitrofying aromatic hydrocarbon chloride, innovation
Point is：Aromatic hydrocarbon chloride and solid acid catalyst are put into reaction vessel, and anhydrous cupric sulfate then is added or other are similar
Sulfate is stirred continuously, and after stirring evenly, then fuming nitric aicd is slowly added dropwise, and then keeps the temperature 1~5 hour at 55~75 DEG C, is protected
It after temperature, is separated by solid-liquid separation, the solid after separation melts down drying, recycles；Liquid is washed with hot water, is then tied naturally
It is brilliant to obtain product.
Further, the solid acid catalyst is benzenephosphonic acid or basic zirconium phosphate.
Further, the anhydrous cupric sulfate or other similar to sulfate addition be aromatic hydrocarbon chloride 1~15%,
Most preferably 3~8%.
Further, the fuming nitric aicd and the material ratio of aromatic hydrocarbon chloride are 1~10:1, best material ratio is 2~5:
1。
Further, purity >=99.8% of the product, conversion rate of products >=95%.
The advantage of the invention is that：
（1）The method of nitrofying aromatic hydrocarbon chloride of the present invention, by selecting suitable solid acid catalyst to carry out nitration reaction,
So that product purity and conversion ratio are further promoted, and solid acid can recycle, and not generate waste substantially, compound
Environmentally protective theory；
（2）The method of nitrofying aromatic hydrocarbon chloride of the present invention, solid acid catalyst is using benzenephosphonic acid or basic zirconium phosphate, phosphniline
Sour zirconium or phosphonic acids zirconium have good phase transfer effect and strong acid effect, acid tens of thousands of times stronger than sulfuric acid.
Specific implementation mode
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among the embodiment described range.
Embodiment 1
1mol paracide and benzenephosphonic acid are put into reaction vessel, then heating and melting is added 1g anhydrous cupric sulfates, stirs
After mixing uniformly, the fuming nitric aicd of 2.0mol is slowly added dropwise, then keeps the temperature 3 hours at 65 DEG C, after heat preservation, carries out solid-liquid point
From the solid after separation melts down drying, recycles；Liquid is washed with hot water, and then spontaneous nucleation obtains product, the purity of product
Up to 99.82%, conversion rate of products 95.6%.
Embodiment 2
1mol paracide and basic zirconium phosphate are put into reaction vessel, then heating and melting is added 1g anhydrous cupric sulfates, stirs
After mixing uniformly, the fuming nitric aicd of 2.0mol is slowly added dropwise, then keeps the temperature 2 hours at 75 DEG C, after heat preservation, carries out solid-liquid point
From the solid after separation melts down drying, recycles；Liquid is washed with hot water, and then spontaneous nucleation obtains product, the purity of product
Up to 99.83%, conversion rate of products 95.8%.
Embodiment 3
1mol paracide and basic zirconium phosphate are put into reaction vessel, then heating and melting is added 1g anhydrous cupric sulfates, stirs
After mixing uniformly, the fuming nitric aicd of 3.5mol is slowly added dropwise, then keeps the temperature 2.5 hours at 70 DEG C, after heat preservation, carries out solid-liquid
Separation, the solid after separation melt down drying, recycle；Liquid is washed with hot water, and then spontaneous nucleation obtains product, product it is pure
Degree is up to 99.87%, conversion rate of products 96.1%.
The basic principles and main features and advantages of the present invention of the present invention have been shown and described above.The skill of the industry
Art personnel it should be appreciated that the present invention is not limited to the above embodiments, the above embodiments and description only describe
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (4)
1. a kind of method of nitrofying aromatic hydrocarbon chloride, it is characterised in that：Aromatic hydrocarbon chloride and solid acid are put into reaction vessel
Then anhydrous cupric sulfate is added in catalyst, be stirred continuously, and after stirring evenly, then fuming nitric aicd is slowly added dropwise, then 55~75
1~5 hour is kept the temperature at DEG C, after heat preservation, is separated by solid-liquid separation, the solid after separation melts down drying, recycles；Liquid is used
Hot water washs, and then spontaneous nucleation obtains product；The solid acid catalyst is benzenephosphonic acid；The addition of the anhydrous cupric sulfate
It is the 1~15% of aromatic hydrocarbon chloride；
The fuming nitric aicd and the material ratio of aromatic hydrocarbon chloride are 1~10:1.
2. the method for nitrofying aromatic hydrocarbon chloride according to claim 1, it is characterised in that：The anhydrous cupric sulfate adds
Enter 3~8% that amount is aromatic hydrocarbon chloride.
3. the method for nitrofying aromatic hydrocarbon chloride according to claim 1, it is characterised in that：The fuming nitric aicd and aromatic hydrocarbons chlorine
The material ratio 2~5 of compound:1.
4. the method for nitrofying aromatic hydrocarbon chloride according to claim 1, it is characterised in that：The purity of the product >=
99.8%, conversion rate of products >=95%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610371878.5A CN106008223B (en) | 2016-05-31 | 2016-05-31 | A kind of method of nitrofying aromatic hydrocarbon chloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610371878.5A CN106008223B (en) | 2016-05-31 | 2016-05-31 | A kind of method of nitrofying aromatic hydrocarbon chloride |
Publications (2)
| Publication Number | Publication Date |
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| CN106008223A CN106008223A (en) | 2016-10-12 |
| CN106008223B true CN106008223B (en) | 2018-08-31 |
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ID=57091578
Family Applications (1)
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| CN201610371878.5A Active CN106008223B (en) | 2016-05-31 | 2016-05-31 | A kind of method of nitrofying aromatic hydrocarbon chloride |
Country Status (1)
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Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102004035742A1 (en) * | 2004-07-23 | 2006-03-16 | Skw Stickstoffwerke Piesteritz Gmbh | N-phenylphosphoric triamides, processes for their preparation and their use as agents for regulating or inhibiting enzymatic urea hydrolysis |
| CN100457710C (en) * | 2004-12-01 | 2009-02-04 | 微宏科技（湖州）有限公司 | Metal salt catalyzed benzene nitrating to prepare nitrobenzene |
| CN102260174B (en) * | 2011-06-28 | 2013-12-11 | 江苏隆昌化工有限公司 | Application of solid acid catalyst in preparation of 2,5-dichloronitrobenzene |
| CN103408429B (en) * | 2013-08-15 | 2015-07-08 | 江苏隆昌化工有限公司 | Method for nitration synthesis of nitrobenzene under catalysis of strong acid-type ZSM-5 molecular sieve |
| CN104230716A (en) * | 2014-08-28 | 2014-12-24 | 厦门大学 | Method for enhancing nitration reaction rate of 2,5-dichloronitrobenzene |
| CN105152936B (en) * | 2015-09-14 | 2017-10-10 | 江苏隆昌化工有限公司 | A kind of method that solid acid catalysis nitrifies paracide |
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