CN107098830A - A kind of refined process of salicylonitrile - Google Patents
A kind of refined process of salicylonitrile Download PDFInfo
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- CN107098830A CN107098830A CN201710241380.1A CN201710241380A CN107098830A CN 107098830 A CN107098830 A CN 107098830A CN 201710241380 A CN201710241380 A CN 201710241380A CN 107098830 A CN107098830 A CN 107098830A
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- salicylonitrile
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/32—Separation; Purification; Stabilisation; Use of additives
- C07C253/34—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the process that a kind of salicylonitrile is refined, the process specifically includes following steps：The salicylonitrile input refining kettle that will be refined, adds dimethylbenzene, water and the sodium chloride of metering, is warming up to 90~95 DEG C, half an hour static layering is stirred, oil reservoir is transferred to crystallization kettle by point sub-cloud water, water layer is added to the xylene extraction of metering simultaneously, extract is transferred to crystallization kettle simultaneously；Salicylonitrile of the present invention passes through refined, extraction and crystallization treatment, the impurity in salicylonitrile defective work can effectively be dispelled, will be high compared with yield, quality is recrystallized, present invention optimizes the process design that salicylonitrile is refined, meet the requirement that the refined process of salicylonitrile is designed.
Description
Technical field
The present invention relates to organic compound technical field of refinement, and in particular to a kind of refined process of salicylonitrile.
Background technology
Salicylonitrile, Chinese nickname：Salicylonitrile；2- cyanophenols；2- 4-hydroxy-benzonitriles；O-hydroxy nitrile；Adjacent cyano group
Phenol, physicochemical property：Crystallization；92-95 DEG C of fusing point (102-102.5 DEG C), the greyish white toner powder of 149 DEG C/1.9kPa of boiling point (14mmHg)
Last shape solid, great penetrating odor can allow people's breathing to be affected, smell is pained on a small quantity；If without general under ventilation state
A small amount of salicylonitrile is opened wide, and smell can spread all over whole interior rapidly；Therefore the measure that must be properly protected during operation, reduce to respiratory tract
Stimulation；Intermediate as organic synthesis bunitrolol, bactericide azoxystrobin intermediate.
Salicylonitrile is the intermediate of important organic synthesis bunitrolol, bactericide azoxystrobin intermediate；Existing bigcatkin willow
General precision is relatively low after nitrile synthesis, and many byproducts will be so produced when being reacted with other materials, while can slow down anti-
The speed answered, the yield of reduction production thing.
, mainly based on the exquisite method of recrystallization, there is following ask in the exquisite process of salicylonitrile of the prior art
Topic：
1. the refined salicylonitrile that recrystallizing technology method is obtained, the purity of salicylonitrile does not reach really as organic synthesis cloth
The need for Ni Luoer intermediate, bactericide azoxystrobin intermediate；
2. recrystallizing technology method refines salicylonitrile, the yield of product is unsatisfactory, does not often reach actual industrial product
The need for；
3. there is shadow the refined salicylonitrile that recrystallizing technology method is obtained, inside in the presence of the follow-up commercial Application of more multipair salicylonitrile
Loud impurity, such as sodium chloride.
The content of the invention
To solve the above problems, the present invention proposes a kind of refined process of salicylonitrile.
To realize the object of the invention, the technical scheme of use is：A kind of refined process of salicylonitrile, the technique side
Method specifically includes following steps：
(1) dissolving, the layering of salicylonitriles：The salicylonitrile input refining kettle that will be refined, adds dimethylbenzene, the water of metering
And sodium chloride, 90~95 DEG C are warming up to, half an hour is stirred after stir speed (S.S.) is set, treats that solution stand is layered, under refining kettle
A portion outlet point sub-cloud water, crystallization kettle is transferred to from the lower part outlet of refining kettle by oil reservoir；
(2) is extracted：It will be delivered to from the water layer branched away from the lower part outlet of refining kettle in extraction kettle, in extraction kettle
After the dimethylbenzene for adding metering, set in extraction kettle and extracted after extraction temperature, the extract containing dimethylbenzene and salicylonitrile
Crystallization kettle is transferred to simultaneously, the raffinate containing water is transferred to devil liquor recovery processing system.
(3) is crystallized：The oil reservoir being transferred to from refining kettle and the extract being transferred to from extraction kettle are delivered to crystallization kettle,
Uniformly mixed in crystallization kettle, set in crystallization kettle and crystallized after crystallization mode, obtain refined salicylonitrile product.
It is preferred that, the crystallization mode of described salicylonitrile in crystallization kettle is slow cooling crystallization, cooling scope is 20~
90 DEG C, falling temperature gradient is 0.1~10 DEG C/min.
It is preferred that, the temperature range of described salicylonitrile in refining kettle is specially 92~95 DEG C, and agitating mode is machinery
Stirring, stir speed (S.S.) is 300~500 turns/min.
It is preferred that, it is the step of the process of the recovery and processing system of described raffinate：
(1) distills：Raffinate is transferred to distillation still, boiled off first containing acid low-boiling-point substance, then boils off most of water,
Obtain bottom residue；
(2) is crystallized：The residue that distillation still bottom is obtained is transferred in evaporative crystallization kettle, raises temperature heating crystalline
Kettle, is evaporated crystallization, obtains byproduct.
It is preferred that, described crystallization kettle bottom byproduct is mainly the sodium chloride that purity is 98%.
It is preferred that, described crystallization temperature is 100~800 DEG C, and actual temp scope is 100~300 DEG C.
Compared with prior art, the beneficial effects of the invention are as follows：A kind of refined technique of salicylonitrile involved in the present invention
Method, the process specifically includes following steps：The salicylonitrile input refining kettle that will be refined, adds the diformazan of metering
Benzene, water and sodium chloride, are warming up to 90~95 DEG C, stir half an hour static layering, and oil reservoir is transferred to crystallization kettle by point sub-cloud water,
Water layer is added to the xylene extraction of metering simultaneously, extract is transferred to crystallization kettle simultaneously, with advantages below：
1. the refined process of salicylonitrile of the present invention, by the refined of salicylonitrile, extraction and crystallization treatment,
The impurity in salicylonitrile defective work can be effectively dispelled, will be high compared with yield, quality is recrystallized；
2. the refined process of salicylonitrile of the present invention, can effectively overcome the low of prior art recrystallization presence
The defect of yield and low-purity；
3. the refined process of salicylonitrile of the present invention, the recycling to raffinate is carried out after refined, is obtained
To the sodium chloride that the purity that can be sold as byproduct is 98%, cost can be reduced by selling byproduct, embody economy
And practicality, the refined process design of salicylonitrile is optimized, the requirement of the refined process design of salicylonitrile is met.
Brief description of the drawings
Fig. 1 is the refined process process chart of salicylonitrile of the present invention.
Fig. 2 is the process process chart of the recovery and processing system of raffinate of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Embodiment 1
Refer to shown in Fig. 1, the technical solution adopted by the present invention is：A kind of refined process of salicylonitrile, the work
Process specifically includes following steps：
(1) dissolving, the layering of salicylonitriles：The salicylonitrile input refining kettle that will be refined, adds dimethylbenzene, the water of metering
And sodium chloride, 90~95 DEG C are warming up to, half an hour is stirred after stir speed (S.S.) is set, treats that solution stand is layered, under refining kettle
A portion outlet point sub-cloud water, crystallization kettle is transferred to from the lower part outlet of refining kettle by oil reservoir；
(2) is extracted：It will be delivered to from the water layer branched away from the lower part outlet of refining kettle in extraction kettle, in extraction kettle
After the dimethylbenzene for adding metering, set in extraction kettle and extracted after extraction temperature, the extract containing dimethylbenzene and salicylonitrile
Crystallization kettle is transferred to simultaneously, the raffinate containing water is transferred to devil liquor recovery processing system.
(3) is crystallized：The oil reservoir being transferred to from refining kettle and the extract being transferred to from extraction kettle are delivered to crystallization kettle,
Uniformly mixed in crystallization kettle, set in crystallization kettle and crystallized after crystallization mode, obtain refined salicylonitrile product.
Refer to shown in Fig. 2, the technical solution adopted by the present invention is：A kind of refined process of salicylonitrile, it is described
The step of process of the recovery and processing system of raffinate is：
(1) distills：Raffinate is transferred to distillation still, boiled off first containing acid low-boiling-point substance, then boils off most of water,
Obtain bottom residue；
(2) is crystallized：The residue that distillation still bottom is obtained is transferred in evaporative crystallization kettle, raises temperature heating crystalline
Kettle, is evaporated crystallization, obtains byproduct.
Operation principle：In use, refined underproof salicylonitrile will be needed to put into refining kettle, add as metering
Dimethylbenzene, water and sodium chloride, are warming up to after 90~95 DEG C, stirring half an hour and cause solution stand layering, from refining kettle
Lower part sub-cloud water, remaining oil reservoir in refining kettle is transferred in crystallization kettle；The water layer branched away from refining kettle is added into meter
The dimethylbenzene of amount is extracted in extraction kettle, and extract is transferred into crystallization kettle simultaneously, raffinate is transferred at devil liquor recovery
Reason system；The oil reservoir being transferred to from refining kettle and the extract being transferred to from extraction kettle are uniformly mixed in crystallization kettle, in knot
Crystallized in brilliant kettle.
Further, crystallization mode of the described salicylonitrile in crystallization kettle crystallizes for slow cooling, and cooling scope is 20
~90 DEG C, falling temperature gradient is 0.1~10 DEG C/min.
Further, temperature range of the described salicylonitrile in refining kettle is specially 92~95 DEG C, and agitating mode is machine
Tool is stirred, and stir speed (S.S.) is 300~500 turns/min.
Further, crystallization kettle bottom byproduct is mainly that purity is 98% in the recovery and processing system of described raffinate
Sodium chloride.
Further, crystallization temperature is 100~800 DEG C in crystallization kettle in the recovery and processing system of described raffinate, tool
Temperature scope is 100~300 DEG C.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
1. a kind of refined process of salicylonitrile, it is characterised in that：The process specifically includes following steps：
(1) dissolving, the layering of salicylonitriles：The salicylonitrile input refining kettle that will be refined, adds dimethylbenzene, water and the chlorine of metering
Change sodium, be warming up to 90~95 DEG C, half an hour is stirred after stir speed (S.S.) is set, treat that solution stand is layered, go out from the bottom of refining kettle
Mouthful point sub-cloud water, crystallization kettle is transferred to from the lower part outlet of refining kettle by oil reservoir；
(2) is extracted：It will be delivered in extraction kettle, added in extraction kettle from the water layer branched away from the lower part outlet of refining kettle
After the dimethylbenzene of metering, set in extraction kettle and extracted after extraction temperature, the extract containing dimethylbenzene and salicylonitrile is simultaneously
Crystallization kettle is transferred to, the raffinate containing water is transferred to devil liquor recovery processing system.
(3) is crystallized：The oil reservoir being transferred to from refining kettle and the extract being transferred to from extraction kettle are delivered to crystallization kettle, in knot
Uniformly mixed in brilliant kettle, set in crystallization kettle and crystallized after crystallization mode, obtain refined salicylonitrile product.
2. the refined process of salicylonitrile according to claim 1, it is characterised in that：Described salicylonitrile is in crystallization kettle
Interior crystallization mode crystallizes for slow cooling, and cooling scope is 20~90 DEG C, and falling temperature gradient is 0.1~10 DEG C/min.
3. the refined process of salicylonitrile according to claim 1, it is characterised in that：Described salicylonitrile is in refining kettle
In temperature range be specially 92~95 DEG C, agitating mode be agitator drive mechanical agitation, stir speed (S.S.) be 300~500
Turn/min.
4. the refined process of salicylonitrile according to claim 1, it is characterised in that：At the recovery of described raffinate
The step of process of reason system is：
(1) distills：Raffinate is transferred to distillation still, boiled off first containing acid low-boiling-point substance, then boils off most of water, is obtained
Bottom residue；
(2) is crystallized：The residue that distillation still bottom is obtained is transferred in evaporative crystallization kettle, is raised temperature heating crystalline kettle, is entered
Row evaporative crystallization, obtains byproduct.
5. the refined process of salicylonitrile according to claim 4, it is characterised in that：Described crystallization kettle bottom byproduct
Predominantly purity is 98% sodium chloride.
6. the refined process of salicylonitrile according to claim 4, it is characterised in that：Described crystallization temperature is 100
~800 DEG C, actual temp scope is 100~300 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710241380.1A CN107098830A (en) | 2017-04-13 | 2017-04-13 | A kind of refined process of salicylonitrile |
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| CN201710241380.1A CN107098830A (en) | 2017-04-13 | 2017-04-13 | A kind of refined process of salicylonitrile |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558704A (en) * | 2018-05-29 | 2018-09-21 | 安徽广信农化股份有限公司 | A kind of process of methyl carbamate wastewater treatment |
| CN110818593A (en) * | 2019-11-07 | 2020-02-21 | 湖南化工研究院有限公司 | Refining method of o-hydroxybenzonitrile |
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| EP1289937A1 (en) * | 2000-06-14 | 2003-03-12 | Rhodia Chimie | Method for separating a hydroxybenzonitrile-type compound |
| CN101781235A (en) * | 2010-02-09 | 2010-07-21 | 重庆紫光化工股份有限公司 | Method for preparing 2-cyanophenol |
| CN103739518A (en) * | 2013-12-26 | 2014-04-23 | 安徽广信农化股份有限公司 | Synthesis process for 2-hydroxybenzonitrile |
| CN106008261A (en) * | 2016-05-28 | 2016-10-12 | 安徽广信农化股份有限公司 | Synthesis process of salicylic nitrile used as pesticide intermediate |
| CN106083647A (en) * | 2016-05-28 | 2016-11-09 | 安徽广信农化股份有限公司 | One-step method prepares the synthesis technique of salicylonitrile |
| CN106083655A (en) * | 2016-05-28 | 2016-11-09 | 安徽广信农化股份有限公司 | A kind of novel method for synthesizing of salicylonitrile |
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2017
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| EP1289937A1 (en) * | 2000-06-14 | 2003-03-12 | Rhodia Chimie | Method for separating a hydroxybenzonitrile-type compound |
| US20060149093A1 (en) * | 2000-06-14 | 2006-07-06 | Jean-Francis Spindler | Process for saparating a hydroxybenzonitrile-type compound |
| CN101781235A (en) * | 2010-02-09 | 2010-07-21 | 重庆紫光化工股份有限公司 | Method for preparing 2-cyanophenol |
| CN103739518A (en) * | 2013-12-26 | 2014-04-23 | 安徽广信农化股份有限公司 | Synthesis process for 2-hydroxybenzonitrile |
| CN106008261A (en) * | 2016-05-28 | 2016-10-12 | 安徽广信农化股份有限公司 | Synthesis process of salicylic nitrile used as pesticide intermediate |
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| CN106083655A (en) * | 2016-05-28 | 2016-11-09 | 安徽广信农化股份有限公司 | A kind of novel method for synthesizing of salicylonitrile |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558704A (en) * | 2018-05-29 | 2018-09-21 | 安徽广信农化股份有限公司 | A kind of process of methyl carbamate wastewater treatment |
| CN110818593A (en) * | 2019-11-07 | 2020-02-21 | 湖南化工研究院有限公司 | Refining method of o-hydroxybenzonitrile |
| CN110818593B (en) * | 2019-11-07 | 2022-06-14 | 湖南化工研究院有限公司 | Refining method of o-hydroxybenzonitrile |
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Application publication date: 20170829 |