CN106008261A - Synthesis process of salicylic nitrile used as pesticide intermediate - Google Patents
Synthesis process of salicylic nitrile used as pesticide intermediate Download PDFInfo
- Publication number
- CN106008261A CN106008261A CN201610384296.0A CN201610384296A CN106008261A CN 106008261 A CN106008261 A CN 106008261A CN 201610384296 A CN201610384296 A CN 201610384296A CN 106008261 A CN106008261 A CN 106008261A
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- CN
- China
- Prior art keywords
- phosgene
- tower reactor
- salicylonitrile
- temperature
- distributor
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/20—Preparation of carboxylic acid nitriles by dehydration of carboxylic acid amides
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a synthesis process of salicylic nitrile used as a pesticide intermediate. The synthesis process comprises the steps as follows: (1) adding salicylamide and xylene into a tower reactor, fully dissolving salicylamide, heating the tower reactor temperature, controlling the reaction temperature, introducing phosgene for reaction, and setting a phosgene distributor at the center of the tower reactor; (2) introducing nitrogen in the reactor, connecting a gas outlet with a collecting tank, transferring the resultants in the reactor into a distillation column, respectively collecting fractions at 137-140 DEG C and 145-155 DEG C, cooling and distilling the fraction at the temperature of 137-140 DEG C to obtain xylene, condensing and slicing the fractions at the temperature of 145-155 DEG C to obtain salicyl nitrile. The invention has the advantages of simple process, and the phosgene distributor can greatly improve the effective utilization rate of phosgene; the phosgene unit consumption is decreased from 1.8% to 1.2%. The process is suitable for industrial production.
Description
Technical field
The present invention relates to the synthesis technique of a kind of salicylonitrile, be specifically related in the middle of one used as pesticides
The synthesis technique of the salicylonitrile of body.
Background technology
Salicylonitrile, has another name called salicylonitrile, is a kind of gray powdery solid, great thorn
Swashing property abnormal smells from the patient, people can be allowed on a small quantity to breathe and be affected, abnormal smells from the patient is pained.Salicylonitrile has been commonly used for
Machine the synthesis intermediate of bunitrolol, antibacterial azoxystrobin intermediate.Synthesis about salicylonitrile
Report seldom, mainly has two categories below to react:
First kind reaction is that salicylide first generates Saldox. with hydroxylamine hydrochloride, then passes through acetic anhydride
Or thionyl chloride dehydration obtains salicylonitrile；
Equations of The Second Kind reaction is that salicylamide is de-in the presence of phosgene or thionyl chloride or phosphorus oxychloride
Water, prepares salicylonitrile；
First kind reaction is the salicylonitrile preparation method that domestic application is more, and it can obtain height and contain
Being used as of amount measures the sensitive analysis reagent of Pt, Cu, Zn etc. and for synthetic drug cloth Buddhist nun
The intermediate Saldox. of Luo Er etc..But the method complex operation, the cost of raw material are more expensive, water
The total recovery of poplar nitrile is low, produces substantial amounts of three industrial wastes, is unfavorable for industrialized production.Equations of The Second Kind
Method is amides compound nitrile glycosylation reaction, and this type of reactions steps is simple, quantity of three wastes is few, but
In prior art, in phosgenation reaction, the effective rate of utilization of phosgene is relatively low, and the consumption of phosgene is big not only
Add the probability of plant operations personnel's personal injury, and the later stage of phosgene is processed the most not
Easily, add entreprise cost simultaneously.
Summary of the invention
For problems of the prior art, the present invention provides a kind of as pesticide intermediate
The synthesis technique of salicylonitrile.
The present invention can be achieved through the following technical solutions:
A kind of synthesis technique of the salicylonitrile as pesticide intermediate, synthesis technique step is as follows:
(1) in tower reactor, add the salicylamide of 1 weight portion and the molten of 2 weight portions
Agent dimethylbenzene, after salicylamide fully dissolves, opens jacket steam and carries out tower reactor
Heat up, control temperature and be 90-110 DEG C, lead to from the import department of the bottom phosgene of tower reactor
Enter phosgene and carry out phosgenation reaction, and the middle part of tower reactor arranges phosgene distributor, phosgene
Distributor is connected with the import of phosgene, and gas outlet is arranged at the top of tower reactor；
(2) being filled with nitrogen in tower reactor catches up with gas, gas outlet to be connected with capture tank,
Capture tank top is provided with ammonia spray system, and the middle part of capture tank arranges blower fan, under capture tank
The outlet in portion is connected with scrubbing tower, transfers in rectifying column by the product in tower reactor,
Collecting temperature respectively is 137-140 DEG C and 145-155 DEG C of fraction, is 137-140 DEG C by temperature
Fraction cooling after distill, i.e. obtain solvent xylene, and temperature be that 145-155 DEG C of fraction is cold
Cut into slices after Ning, obtain product salicylonitrile.
Further, the phosgene distributor described in step (1) is to be entered by a key light conductance
Pipe and phosgene distribution looped pipeline composition.
Further, described key light gas ingress pipe is connected with the import of phosgene, and key light conductance
Enter pipe and phosgene distribution looped pipeline is mutually perpendicular to place.
Further, the described uniform fine and close aperture of phosgene distribution looped pipeline top distribution.
The invention have the benefit that 1) by arranging phosgene distributor in the reactor, can
To increase substantially the effective rate of utilization of phosgene so that the unit consumption of phosgene is by 1.8 percentage points of falls
To 1.2 percentage points；2) by arranging ammonia spray system on the top of capture tank, permissible
Effectively absorbing hydrogen chloride and phosgene, it is to avoid leaking of toxic gas, simultaneously blower fan arrange permissible
Making mixed gas be upwardly into spray system to be absorbed, impurity will return from the bottom of capture tank
In scrubbing tower, so may insure that the quality of gas, thus beneficially the recycling of raw material.
Detailed description of the invention:
By embodiment, the detailed description of the invention of the present invention is made an explanation below.
Embodiment
The invention provides the synthesis technique of a kind of salicylonitrile as pesticide intermediate, synthesize work
Skill step is as follows: (1) adds salicylamide and 2 weight of 1 weight portion in tower reactor
The solvent xylene of part, after salicylamide fully dissolves, opens jacket steam to tower reaction
Device heats up, and controlling temperature is 105 DEG C, from the import department of the bottom phosgene of tower reactor
It is passed through phosgene and carries out phosgenation reaction, and the middle part of tower reactor arranges phosgene distributor, light
Gas distributor is connected with the import of phosgene, and phosgene distributor be by a key light gas ingress pipe and
Phosgene distribution looped pipeline composition, key light gas ingress pipe and phosgene distribution looped pipeline are to be mutually perpendicular to place
, and uniform point of phosgene distribution looped pipeline top distribution uniform fine and close aperture, beneficially phosgene
Cloth, thus increase substantially the effective rate of utilization of phosgene, the top of tower reactor also has gas
Outlet；(2) being filled with nitrogen in tower reactor catches up with gas, gas outlet to be connected with capture tank,
Capture tank top is provided with ammonia spray system, can absorb phosgene and hydrogen chloride gas, trapping
The middle part of tank arranges blower fan, is conveyed upwards into mixed gas in ammonia spray system processing, catches
The outlet of collection tank bottom is connected with scrubbing tower, so may insure that the purity of mixed gas；Again will
Product in tower reactor is transferred in rectifying column, collects temperature respectively and is 137-140 DEG C
With 145-155 DEG C of fraction, distill after the fraction that temperature is 137-140 DEG C is cooled down, i.e. obtain
Solvent xylene, and temperature is section after 145-155 DEG C of fraction condensation, obtains product salicylonitrile.
The invention have the benefit that 1) by arranging phosgene distributor in the reactor, can
To increase substantially the effective rate of utilization of phosgene so that the unit consumption of phosgene is by 1.8 percentage points of falls
To 1.2 percentage points；2) by arranging ammonia spray system on the top of capture tank, permissible
Effectively absorbing hydrogen chloride and phosgene, it is to avoid leaking of toxic gas, simultaneously blower fan arrange permissible
Making mixed gas be upwardly into spray system to be absorbed, impurity will return from the bottom of capture tank
In scrubbing tower, so may insure that the quality of gas, thus beneficially the recycling of raw material.
The foregoing is only highly preferred embodiment of the present invention, not in order to limit the present invention, all
Any amendment, equivalent and the improvement etc. made within the spirit and principles in the present invention, all should
Within being included in protection scope of the present invention.
Claims (4)
1. the synthesis technique of the salicylonitrile being used as pesticide intermediate, it is characterised in that close
Become processing step as follows:
(1) in tower reactor, add the salicylamide of 1 weight portion and the molten of 2 weight portions
Agent dimethylbenzene, after salicylamide fully dissolves, opens jacket steam and carries out tower reactor
Heat up, control temperature and be 90-110 DEG C, lead to from the import department of the bottom phosgene of tower reactor
Enter phosgene and carry out phosgenation reaction, and the middle part of tower reactor arranges phosgene distributor, phosgene
Distributor is connected with the import of phosgene, and gas outlet is arranged at the top of tower reactor；
(2) being filled with nitrogen in tower reactor catches up with gas, gas outlet to be connected with capture tank,
Capture tank top is provided with ammonia spray system, and the middle part of capture tank arranges blower fan, under capture tank
The outlet in portion is connected with scrubbing tower, transfers in rectifying column by the product in tower reactor,
Collecting temperature respectively is 137-140 DEG C and 145-155 DEG C of fraction, is 137-140 DEG C by temperature
Fraction cooling after distill, i.e. obtain solvent xylene, and temperature be that 145-155 DEG C of fraction is cold
Cut into slices after Ning, obtain product salicylonitrile.
The synthesis of a kind of salicylonitrile as pesticide intermediate the most according to claim 1
Technique, it is characterised in that the phosgene distributor described in step 1 is to be entered by a key light conductance
Pipe and phosgene distribution looped pipeline composition.
The synthesis of a kind of salicylonitrile as pesticide intermediate the most according to claim 2
Technique, it is characterised in that described key light gas ingress pipe is connected with the import of phosgene, and key light
Gas ingress pipe and phosgene distribution looped pipeline are mutually perpendicular to place.
The synthesis of a kind of salicylonitrile as pesticide intermediate the most according to claim 2
Technique, it is characterised in that the described uniform fine and close aperture of phosgene distribution looped pipeline top distribution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610384296.0A CN106008261A (en) | 2016-05-28 | 2016-05-28 | Synthesis process of salicylic nitrile used as pesticide intermediate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610384296.0A CN106008261A (en) | 2016-05-28 | 2016-05-28 | Synthesis process of salicylic nitrile used as pesticide intermediate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106008261A true CN106008261A (en) | 2016-10-12 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610384296.0A Pending CN106008261A (en) | 2016-05-28 | 2016-05-28 | Synthesis process of salicylic nitrile used as pesticide intermediate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098830A (en) * | 2017-04-13 | 2017-08-29 | 安徽广信农化股份有限公司 | A kind of refined process of salicylonitrile |
| CN114853631A (en) * | 2022-06-08 | 2022-08-05 | 江苏常隆农化有限公司 | Process for continuously synthesizing salicylanitrile by phosgene method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204365263U (en) * | 2014-12-02 | 2015-06-03 | 安徽东至广信农化有限公司 | A kind of salicylonitrile phosgene reaction tail gas collecting device |
| CN105152972A (en) * | 2015-09-28 | 2015-12-16 | 湖南国发精细化工科技有限公司 | Method for synthesizing o-hydoxybenzonitrile |
| CN105195080A (en) * | 2015-10-10 | 2015-12-30 | 开封华瑞化工新材料股份有限公司 | Synthesis device and method for xylylene diisocynate |
-
2016
- 2016-05-28 CN CN201610384296.0A patent/CN106008261A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204365263U (en) * | 2014-12-02 | 2015-06-03 | 安徽东至广信农化有限公司 | A kind of salicylonitrile phosgene reaction tail gas collecting device |
| CN105152972A (en) * | 2015-09-28 | 2015-12-16 | 湖南国发精细化工科技有限公司 | Method for synthesizing o-hydoxybenzonitrile |
| CN105195080A (en) * | 2015-10-10 | 2015-12-30 | 开封华瑞化工新材料股份有限公司 | Synthesis device and method for xylylene diisocynate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098830A (en) * | 2017-04-13 | 2017-08-29 | 安徽广信农化股份有限公司 | A kind of refined process of salicylonitrile |
| CN114853631A (en) * | 2022-06-08 | 2022-08-05 | 江苏常隆农化有限公司 | Process for continuously synthesizing salicylanitrile by phosgene method |
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Application publication date: 20161012 |
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