CN110305060A - A kind of 2- chloro-5-trichloromethylpyridine rectification and purification method and device - Google Patents
A kind of 2- chloro-5-trichloromethylpyridine rectification and purification method and device Download PDFInfo
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- CN110305060A CN110305060A CN201910659221.2A CN201910659221A CN110305060A CN 110305060 A CN110305060 A CN 110305060A CN 201910659221 A CN201910659221 A CN 201910659221A CN 110305060 A CN110305060 A CN 110305060A
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- chloro
- reaction kettle
- trichloromethylpyridine
- rectification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D213/61—Halogen atoms or nitro radicals
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- Chemical Kinetics & Catalysis (AREA)
- Pyridine Compounds (AREA)
Abstract
The present invention discloses a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method and device, 2- chloro-5-trichloromethylpyridine rectification and purification is carried out by the device in 2- chloro-5-trichloromethylpyridine rectification and purification, a kind of device for 2- chloro-5-trichloromethylpyridine rectification and purification provided by the invention can efficiently carry out the purification of 2- chloro-5-trichloromethylpyridine crude product, apparatus structure is simple, it is at low cost, the method of purification for cooperating 2- chloro-5-trichloromethylpyridine crude product, can greatly improve the purification rate of 2- chloro-5-trichloromethylpyridine crude product.
Description
Technical field
The present invention relates to medicine and pesticide intermediate technical fields, and in particular to a kind of 2- chloro-5-trichloromethylpyridine essence
Evaporate method of purification and device.
Background technique
2- chloro-5-trichloromethylpyridine is a kind of very important medicine and pesticide intermediate, can be used for preparing pharmaceuticals,
Agricultural chemicals and biological agent etc., especially synthesizing efficient new pesticide haloxyfop, imidacloprid level-one contain chloropyridines
The vital intermediate of novel pesticide, with the new varieties of pesticides containing chloropyridines of 2- chloro-5-trichloromethylpyridine synthesis in state
The inside and outside development and exploitation just obtained energetically, however more by-product can be generated in 2- chloro-5-trichloromethylpyridine preparation process
Object needs to carry out purification processes, to improve the purity of 2- chloro-5-trichloromethylpyridine.
Summary of the invention
The object of the present invention is to provide a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method and devices, to improve 2-
Purity when chloro-5-trichloromethylpyridine produces.
The present invention is achieved by the following technical solutions.
A kind of device for 2- chloro-5-trichloromethylpyridine rectification and purification, including supporting leg, reaction kettle ontology, reaction kettle
Upper cover, agitating paddle, discharge port, heating chamber, stirring motor and feed inlet, the reaction kettle ontology upper end setting with reaction kettle on
Lid, and reaction kettle body bottom portion is fixed on supporting leg, reaction kettle upper cover upper end offers feed inlet, and the reaction of feed inlet side
Exhaust outlet is communicated on kettle on lid, is provided with air inlet on the left of reaction kettle upper cover, and Gai Shangan on the reaction kettle on the right side of air inlet
Equipped with pressure gauge, it is fixed with stirring motor in the middle part of reaction kettle upper cover, and stirring motor is internally provided with agitating paddle phase with reaction chamber
Even, it reacts and temperature sensor is installed on cavity wall, and be enclosed with heating chamber on the outside of reaction chamber, supporting leg bottom is equipped with discharging
Mouthful.
As further technical solution, the air inlet and exhaust outlet have air valve, and set above reaction kettle upper cover
Sealing cover is installed on the feed inlet set, and control valve is installed on the discharge port being arranged below reaction kettle ontology.
It as further technical solution, is heated in the heating chamber for hot-oil circulation, and the heat after heating equipment heating
Oil is entered after heating chamber by the heating import below heating chamber and is output to by the heating exit being arranged above heating chamber
Heating equipment.
As further technical solution, the observation window of transparent material, and observation window are provided on the reaction kettle ontology
It is not connected to across reaction kettle ontology with reaction kettle ontology, and is provided with graduation mark on the outside of observation window.
A kind of 2- chloro-5-trichloromethylpyridine rectification and purification method, the 2- that 15.6-17g is added into reaction kettle ontology are chloro-
5- picoline crude product, 0.1-0.15g methylethyl ketone peroxide, 50-60mL o-dichlorohenzene, are passed through nitrogen, are stirred with 150r/min revolving speed
10-15min is mixed, is warming up to 80 DEG C, stops logical nitrogen and switches to be passed through chlorine, be continuously heating to 142 DEG C, under constant temperature, chlorine drum
Bubble reacts, and in reaction process, 0.07-0.075g methylethyl ketone peroxide was added every 2 hours and stops heating after reaction 20 hours, stops
It is only passed through chlorine, is passed through nitrogen, bubbling catches up with chlorine 1 hour, after reaction solution is evaporated under reduced pressure precipitation, separation elution, with dehydrated alcohol pair
After obtained product is recrystallized, vacuum drying obtains the solid 2- chloro-5-trichloromethylpyridine of white.
As further technical solution, separation carries out column chromatography progress using with silica GF254 in the separation elution.
As further technical solution, the eluant, eluent group that use is eluted in the separation elution becomes V (ethyl acetate):
V (petroleum ether)=1:20.
2- chloro-5-trichloromethylpyridine is carried out by using the device for 2- chloro-5-trichloromethylpyridine rectification and purification
Rectification and purification.
From the above technical scheme, it can be seen that the beneficial effects of the present invention are:
A kind of device for 2- chloro-5-trichloromethylpyridine rectification and purification provided by the invention can efficiently carry out 2-
The purification of chloro-5-trichloromethylpyridine crude product, apparatus structure is simple, at low cost, cooperation 2- chloro-5-trichloromethylpyridine crude product
Method of purification, can greatly improve the purification rate of 2- chloro-5-trichloromethylpyridine crude product, to significantly eliminate 2-
Impurity content in chloro-5-trichloromethylpyridine crude product improves the purity of 2- chloro-5-trichloromethylpyridine product, improves 2-
The quality of chloro-5-trichloromethylpyridine product has significant economic benefit.
Detailed description of the invention
A kind of appearance diagram of device for 2- chloro-5-trichloromethylpyridine rectification and purification Fig. 1 of the invention；
A kind of appearance diagram of device for 2- chloro-5-trichloromethylpyridine rectification and purification Fig. 2 of the invention.
In figure: 1, supporting leg；2, reaction kettle ontology；3, reaction kettle upper cover；4, observation window；5, graduation mark；6, reaction chamber；7, it stirs
Mix paddle；8, discharge port；9, import is heated；10, temperature sensor；11, heating chamber；12, air inlet；13, pressure gauge；14, it stirs
Motor；15, feed inlet；16, exhaust outlet；17, heating exit.
Specific embodiment
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.Reality used in the examples
The condition of applying can be for further adjustments according to the condition of producer, and unaccounted implementation condition is usually conventional laboratory conditions.
Embodiment 1
The chloro- 5- of 2- of 15.6g is added into reaction kettle ontology for a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method
Picoline crude product, 0.1g methylethyl ketone peroxide, 50mL o-dichlorohenzene, are passed through nitrogen, stir 10min with 150r/min revolving speed, rise
Temperature stops logical nitrogen and switches to be passed through chlorine, be continuously heating to 142 DEG C, under constant temperature, chlorine blistering reaction reacted to 80 DEG C
Cheng Zhong added 0.07g methylethyl ketone peroxide every 2 hours, after reaction 20 hours, stopped heating, stopping is passed through chlorine, is passed through nitrogen
Gas, bubbling catch up with chlorine 1 hour, and after reaction solution is evaporated under reduced pressure precipitation, separation elution ties obtained product with dehydrated alcohol again
After crystalline substance, vacuum drying obtains the solid 2- chloro-5-trichloromethylpyridine of white.
As further technical solution, separation carries out column chromatography progress using with silica GF254 in the separation elution.
As further technical solution, the eluant, eluent group that use is eluted in the separation elution becomes V (ethyl acetate):
V (petroleum ether)=1:20.
Embodiment 2
The chloro- 5- first of 2- of 17g is added into reaction kettle ontology for a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method
Yl pyridines crude product, 0.15g methylethyl ketone peroxide, 60mL o-dichlorohenzene, are passed through nitrogen, stir 15min, heating with 150r/min revolving speed
To 80 DEG C, stop logical nitrogen and switch to be passed through chlorine, is continuously heating to 142 DEG C, under constant temperature, chlorine blistering reaction, reaction process
In, 0.075g methylethyl ketone peroxide to be added every 2 hours, after reaction 20 hours, stopped heating, stopping is passed through chlorine, is passed through nitrogen,
Bubbling catches up with chlorine 1 hour, and after reaction solution is evaporated under reduced pressure precipitation, separation elution recrystallizes obtained product with dehydrated alcohol
Afterwards, it is dried in vacuo, obtains the solid 2- chloro-5-trichloromethylpyridine of white.
As further technical solution, separation carries out column chromatography progress using with silica GF254 in the separation elution.
As further technical solution, the eluant, eluent group that use is eluted in the separation elution becomes V (ethyl acetate):
V (petroleum ether)=1:20.
Embodiment 3
The chloro- 5- first of 2- of 16g is added into reaction kettle ontology for a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method
Yl pyridines crude product, 0.12g methylethyl ketone peroxide, 55mL o-dichlorohenzene, are passed through nitrogen, stir 12min, heating with 150r/min revolving speed
To 80 DEG C, stop logical nitrogen and switch to be passed through chlorine, is continuously heating to 142 DEG C, under constant temperature, chlorine blistering reaction, reaction process
In, 0.073g methylethyl ketone peroxide to be added every 2 hours, after reaction 20 hours, stopped heating, stopping is passed through chlorine, is passed through nitrogen,
Bubbling catches up with chlorine 1 hour, and after reaction solution is evaporated under reduced pressure precipitation, separation elution recrystallizes obtained product with dehydrated alcohol
Afterwards, it is dried in vacuo, obtains the solid 2- chloro-5-trichloromethylpyridine of white.
As further technical solution, separation carries out column chromatography progress using with silica GF254 in the separation elution.
As further technical solution, the eluant, eluent group that use is eluted in the separation elution becomes V (ethyl acetate):
V (petroleum ether)=1:20.
As shown in Figure 1, a kind of device for 2- chloro-5-trichloromethylpyridine rectification and purification, including reaction kettle ontology 1,
Feed inlet 2, air inlet 3, thermometer 4, motor 5, agitating paddle 6, heating chamber 7, stabilizer blade 8, discharge port 9；The setting of feed inlet 2 exists
1 top of reaction kettle ontology, the air inlet 3 are arranged on the left of 1 top feed mouth of reaction kettle ontology, and the motor 5 is arranged anti-
It answers on the right side of 1 top feed mouth of kettle ontology, the agitating paddle 6 is arranged inside reaction kettle ontology 1, and agitating paddle 6 is connected to motor 5,
Thermometer 4 is provided on the right side of 1 inner wall of reaction kettle ontology, 1 outer wall of reaction kettle ontology is provided with heating chamber 7, described anti-
1 bottom of kettle ontology is answered to be provided with discharge port 9.
As further technical solution, the air inlet 3 has air valve.
As further technical solution, heated in the heating chamber 7 for hot-oil circulation.
Comparative example 1: it is only that in reaction process with the difference of embodiment 1, does not add 0.07-0.075g methylethyl ketone peroxide.
Comparative example 2: it is only that eluant, eluent group becomes V (ethyl acetate) with the difference of embodiment 1: V (petroleum ether)=1:10.
Test
To 2- chloro-5-trichloromethylpyridine purity after embodiment and comparative example 2- chloro-5-trichloromethylpyridine rectification and purification
Compare (2- chloro-5-trichloromethylpyridine crude product purity is 82.1%):
Table 1
| Purity % | |
| Embodiment 1 | 98.2 |
| Embodiment 2 | 98.8 |
| Embodiment 3 | 98.5 |
| Comparative example 1 | 92.3 |
| Comparative example 2 | 96.9 |
As can be seen from Table 1, after the method for the present invention is to 2- chloro-5-trichloromethylpyridine crude product rectification and purification, purity has
It is greatly improved.
Certainly, the above description is not a limitation of the present invention, and the present invention is also not limited to the example above, the art
Those of ordinary skill, within the essential scope of the present invention, variation, change, addition or the replacement made all should belong to the present invention
Protection scope.
Claims (7)
1. a kind of device for 2- chloro-5-trichloromethylpyridine rectification and purification, which is characterized in that including supporting leg (1), reaction kettle
Ontology (2), reaction kettle upper cover (3), agitating paddle (7), discharge port (8), heating chamber (11), stirring motor (14) and feed inlet
(15), reaction kettle ontology (2) the upper end setting and reaction kettle upper cover (3), and reaction kettle ontology (2) bottom is fixed on supporting leg
(1) on, reaction kettle upper cover (3) upper end is offered feed inlet (15), and is connected in the reaction kettle upper cover (3) of feed inlet (15) side
Have exhaust outlet (16), is provided with air inlet (12) on the left of reaction kettle upper cover (3), and the reaction kettle upper cover on the right side of air inlet (12)
(3) it is equipped on pressure gauge (13), is fixed with stirring motor (14) in the middle part of reaction kettle upper cover (3), and stirring motor (14) and anti-
It answers chamber (6) to be internally provided with agitating paddle (7) to be connected, be equipped with temperature sensor (10) on reaction chamber (6) inner wall, and reaction chamber
(6) outside is enclosed with heating chamber (11), and supporting leg (1) bottom is equipped with discharge port (8).
2. being used for the device of 2- chloro-5-trichloromethylpyridine rectification and purification as described in claim 1, it is characterised in that: described
Air inlet (12) and exhaust outlet (16) have air valve, and are equipped on the feed inlet (15) being arranged above reaction kettle upper cover (3)
Sealing cover, and control valve is installed on the discharge port (8) being arranged below reaction kettle ontology (2).
3. being used for the device of 2- chloro-5-trichloromethylpyridine rectification and purification as described in claim 1, it is characterised in that: described
It is heated in heating chamber (11) for hot-oil circulation, and the hot oil after heating equipment heating passes through the heating import below heating chamber (11)
(9) it enters after heating chamber (11) and heating equipment is output to by the heating exit (17) being arranged above heating chamber (11).
4. being used for the device of 2- chloro-5-trichloromethylpyridine rectification and purification as described in claim 1, it is characterised in that: described
The observation window (4) of transparent material is provided on reaction kettle ontology (2), and observation window (4) passes through reaction kettle ontology (2) and reaction kettle
Ontology (2) is not connected to, and is provided with graduation mark (5) on the outside of observation window (4).
5. a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method, it is characterised in that: be added in reaction kettle ontology (2)
Chloro--methylpyridine crude product, 0.1-0.15g methylethyl ketone peroxide, the 50-60mL o-dichlorohenzene of 15.6-17g, is passed through nitrogen, with
150r/min revolving speed stirs 10-15min, is warming up to 80 DEG C, stops logical nitrogen and switches to be passed through chlorine, be continuously heating to 142 DEG C,
Under constant temperature, in reaction process, 0.07-0.075g methylethyl ketone peroxide was added every 2 hours, is reacted 20 hours for chlorine blistering reaction
Afterwards, stop heating, stopping is passed through chlorine, is passed through nitrogen, and bubbling catches up with chlorine 1 hour, and after reaction solution is evaporated under reduced pressure precipitation, separation is washed
De-, after being recrystallized with dehydrated alcohol to obtained product, vacuum drying obtains the solid 2- chloro-5-trichloromethylpyridine of white.
6. a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method as claimed in claim 5, it is characterised in that: described point
Column chromatography progress is carried out using with silica GF254 from separation in elution.
7. a kind of 2- chloro-5-trichloromethylpyridine rectification and purification method as described in claim 1, it is characterised in that: described point
Become V (ethyl acetate) from the eluant, eluent group for eluting use in elution: V (petroleum ether)=1:20.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910659221.2A CN110305060A (en) | 2019-07-22 | 2019-07-22 | A kind of 2- chloro-5-trichloromethylpyridine rectification and purification method and device |
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| CN201910659221.2A CN110305060A (en) | 2019-07-22 | 2019-07-22 | A kind of 2- chloro-5-trichloromethylpyridine rectification and purification method and device |
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|---|---|---|---|---|
| CN103058918A (en) * | 2012-11-30 | 2013-04-24 | 江苏扬农化工股份有限公司 | Method for synthesizing 2-chlorine-5-nitrapyrin and 2, 3-dichloro-5-nitrapyrin |
| CN103787960A (en) * | 2014-02-27 | 2014-05-14 | 江苏省激素研究所股份有限公司 | Synthetic method of 2-chloro-5-trichloromethyl pyridine |
| CN107824141A (en) * | 2017-11-20 | 2018-03-23 | 盐城恒泽水环境治理有限公司 | Reactor |
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| CN108970568A (en) * | 2018-09-18 | 2018-12-11 | 南京华阜信息科技有限公司 | A kind of highly effective reaction kettle |
| CN208356772U (en) * | 2018-05-10 | 2019-01-11 | 攀枝花市吉源科技有限责任公司 | A kind of intelligence polycarboxylate water-reducer reaction kettle |
| CN208554119U (en) * | 2018-05-08 | 2019-03-01 | 江苏金马油脂科技发展有限公司 | A kind of dimeric dibasic acid reaction kettle |
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2019
- 2019-07-22 CN CN201910659221.2A patent/CN110305060A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058918A (en) * | 2012-11-30 | 2013-04-24 | 江苏扬农化工股份有限公司 | Method for synthesizing 2-chlorine-5-nitrapyrin and 2, 3-dichloro-5-nitrapyrin |
| CN103787960A (en) * | 2014-02-27 | 2014-05-14 | 江苏省激素研究所股份有限公司 | Synthetic method of 2-chloro-5-trichloromethyl pyridine |
| CN107824141A (en) * | 2017-11-20 | 2018-03-23 | 盐城恒泽水环境治理有限公司 | Reactor |
| CN208554119U (en) * | 2018-05-08 | 2019-03-01 | 江苏金马油脂科技发展有限公司 | A kind of dimeric dibasic acid reaction kettle |
| CN208356772U (en) * | 2018-05-10 | 2019-01-11 | 攀枝花市吉源科技有限责任公司 | A kind of intelligence polycarboxylate water-reducer reaction kettle |
| CN108786700A (en) * | 2018-06-13 | 2018-11-13 | 运城学院 | A kind of chemosynthesis reaction kettle |
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