CN105254583A - Method for preparing 2-chloro-5-chloromethylthiazole by jet loop reactor - Google Patents

Method for preparing 2-chloro-5-chloromethylthiazole by jet loop reactor Download PDF

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CN105254583A
CN105254583A CN201510804779.7A CN201510804779A CN105254583A CN 105254583 A CN105254583 A CN 105254583A CN 201510804779 A CN201510804779 A CN 201510804779A CN 105254583 A CN105254583 A CN 105254583A
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chloro
reactor
injector
chloromethyl thiazole
chlorine
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CN105254583B (en
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宋建华
史三冬
柳海营
周梁
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Hebei Brilliant Chemical Co Ltd
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Hebei Brilliant Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D277/00Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
    • C07D277/02Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings not condensed with other rings
    • C07D277/20Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
    • C07D277/32Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members 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

Abstract

The invention discloses a method for preparing 2-chloro-5-chloromethylthiazole by a jet loop reactor, and relates to the technical field of synthesis of the 2-chloro-5-chloromethylthiazole. The jet loop reactor comprises an ejector, wherein the ejector is arranged at the upper part of the reaction kettle; a lower outlet of the reaction kettle is communicated with an inlet of a circulating pump; an outlet of the circulating pump is communicated with the inlet of a heat exchanger; the outlet of the heat exchanger is communicated with the top inlet of the ejector; an air inlet pipe is arranged on the side surface of the ejector; 1-isothiocyano-2-chlorine-2-propylene is dissolved into an inert organic solvent to prepare a liquid-phase material; the liquid-phase material is added to the reaction kettle, and enters from the top inlet of the ejector after passing through the circulating pump and the heat exchanger; chlorine enters the ejector through the air inlet pipe and is mixed with the liquid-phase material; the mixed material passes through the reaction kettle, the circulating pump and the heat exchanger and then returns to the top inlet of the ejector; circular reaction is carried out until the chlorine is introduced; a 2-chloro-5-chloromethylthiazole product is obtained after post-treatment. The method disclosed by the invention is high in yield, few in solid wastes and high in production efficiency; the reaction temperature is easy to control.

Description

Injection circulation reactor is utilized to prepare the method for 2-chloro-5-chloromethyl thiazole
Technical field
The present invention relates to 2-chloro-5-chloromethyl thiazole synthesis technical field.
Background technology
2-chloro-5-chloromethyl thiazole (2-Chloro-5-chloromethylthiazole) is the important intermediate of producing the products such as Diacloden, clothianidin, MTI-446 and medicine.
According to the documents such as CN00811445, CN01809972, CN96117934, CN97109983, CN200410056641, CN200780002281, CN201410045648, CN201410045781, CN201410098099-2, CN201410308830.There is number of ways can synthesize 2-chloro-5-chloromethyl thiazole at present, according to raw materials used difference, be mainly divided into following several:
(1) the acrylonitrile-chlorinated method of 1-isothiocyanic acid base-2-: the chloroformic solution of chlorine (maybe can produce the compound of chlorine, as sulfuryl chloride) and 1-isothiocyanic acid base-2-propylene is injected in the chloroform of backflow simultaneously and reacts.The chlorine that this reaction needed is excessive in a large number, side reaction is more, and crude product purity is 41.1%, and the purity after simple distillation is also only 47.8%, yield 50.4%.Just sterling need can be obtained by rectifying.Although this synthetic method process is simple, pass into a large amount of chlorine and easily pollute, the waste of cost, and the yield of product is very low, by product is more.
(2) 1-isothiocyanic acid base-2-chloro-2-propene chlorination process: pass into chlorine under ice bath (or water-bath) cooling in the chloroformic solution of 1-isothiocyanic acid base-2-chloro-2-propene, then temperature controls less than 40 DEG C reactions, until heat release stops.This method will use a large amount of excessive chlorine, and when suitability for industrialized production, if tank reactor gas-liquid mixed uniformity coefficient is poor, side reaction is more, and solid waste is many, and yield is low only has 50-65%; Meanwhile, very high to the control overflow of temperature of reaction, and in reaction process, a large amount of heat release, is difficult to control in Industrial processes.
(3) 1-isothiocyanic acid base-2-chloro-2-propene chlorination process: drip sulfuryl chloride under ice bath (or water-bath) cooling in the chloroformic solution of 1-isothiocyanic acid base-2-chloro-2-propene, then temperature controls less than 80 DEG C reactions, until HCl and SO 2drain rear stopping.The advantage of this method is that side reaction is relatively less, and after distillation, purity can reach more than 98%, yield 80%.But produce a large amount of spent acid and SO in the industrial production 2be difficult to process.
(4) 5-methylene radical-1,3-thiazolidine-2-thio-ketone chlorination process: with chlorine or sulfuryl chloride to 5-methylene radical-1,3-thiazolidine-2-thio-ketone carries out chlorination, can obtain CCT with good yield and purity (yield 72%).But complex manufacturing, cost is high.
Come with some shortcomings all more or less in above-mentioned reaction, such as: the acrylonitrile-chlorinated method of 1-isothiocyanic acid base-2-, in reaction process, side reaction is more, meanwhile, very high to the control overflow of temperature of reaction, and, in reaction process, a large amount of heat release, is difficult to control in Industrial processes.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole, and the method yield is high, and temperature of reaction is easy to control, and side reaction is few, and solid waste is few, and production efficiency is high, is applicable to industrial production.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole, comprises the following steps:
One, injection circulation reactor is adopted, injection circulation reactor comprises reactor, injector, inlet pipe, interchanger and recycle pump, injector is arranged on the top of reactor, the lower part outlet of reactor is connected with the import of recycle pump by pipeline, circulation pump outlet is connected with the import of interchanger by pipeline, the outlet of interchanger is connected with the top entry of injector by pipeline, and the side of injector is provided with inlet pipe, and inlet pipe is provided with air intake valve;
Two, be dissolved in inert organic solvents by 1-isothiocyanic acid base-2-chloro-2-propene and be made into liquid phase material, join in reactor, ON cycle pump, liquid phase material is through recycle pump pressurization, interchanger heat exchange temperature control entering from the top entry of injector; Open air intake valve, gaseous state chlorine enters injector through inlet pipe to carry out mixing and reacting with liquid phase material, mixing the top entry of injector got back to by reacted material after reactor, recycle pump, interchanger, chlorine passes in proportion, after circulating reaction to logical chlorine terminates, obtain the solution containing 2-chloro-5-chloromethyl thiazole;
Three, through aftertreatment precipitation, refining after obtain qualified 2-chloro-5-chloromethyl thiazole product.
Preferably, injector is the venturi-type eductors of jetting type.
Preferably, interchanger is the combination of one or two or more kinds in jacketed still formula interchanger, plate-type heat exchanger or shell and tube heat exchanger.
Preferably, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in inert organic solvents and is made into the liquid phase material that mass concentration is 5% ~ 70%.
Preferably, temperature of reaction is 0-65 DEG C.
Preferred further, temperature of reaction is 10-55 DEG C.
Preferably, ratio is: the final mol ratio of 1-isothiocyanic acid base-2-chloro-2-propene and chlorine is 1:1-1.2.
Preferred further, the final mol ratio of 1-isothiocyanic acid base-2-chloro-2-propene and chlorine is 1:1-1.1.
Preferably, inert organic solvents is selected from toluene, acetonitrile, DMF, chlorobenzene, 1,2-ethylene dichloride, trichloromethane, the mixture of one or two or more kinds in methylene dichloride.
Preferably, aftertreatment precipitation is removed under reduced pressure inert organic solvents, refines as rectification under vacuum or underpressure distillation.
The liquid material mixing efficiency of existing 1-isothiocyanic acid base-2-chloro-2-propene, chlorine technique is low, and uniformity coefficient is poor, and yield is low; Meanwhile, very high to the control overflow of temperature of reaction, and in reaction process, a large amount of heat release, is difficult to control in Industrial processes.
It is vital for mixing for chlorine evaporating method production 2-chloro-5-chloromethyl thiazole fast and effectively.The present invention uses injection circulation reactor, its inner liquid phase jet formed has gas and strong entrainments crushing effect, the mixing efficiency between gas, liquid raw material can be improved, the logical chlorine dose of unit time can be increased, shorten the logical chlorine time, reduce 2-chloro-5-chloromethyl thiazole production cost and 2-chloro-5-chloromethyl thiazole throughput, simultaneously, owing to improve the mixing of storeroom, diffusion, mass-transfer efficiency, resultant of reaction yield is improved, improve 10%-16% than stirred-tank reactor yield.Carry out temperature control by interchanger to reaction mass, and the temperature of reaction required due to present method is interval wide, temperature of reaction is easy to control.
The beneficial effect adopting technique scheme to produce is: the inventive method yield is high, and temperature of reaction is easy to control, and side reaction is few, and solid waste is few, and production efficiency is high, is applicable to industrial production, improves 10%-16% than stirred-tank reactor yield.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation;
Fig. 1 is the structural representation of injection circulation reactor of the present invention;
In figure, 1, reactor; 2, injector; 3, inlet pipe; 4, interchanger; 5, recycle pump.
Embodiment
Embodiments of the invention only illustrate particular case of the invention process, do not limit the present embodiment.
Embodiment 1
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, injection circulation reactor is adopted, as shown in Figure 1, injection circulation reactor comprises reactor 1, injector 2, inlet pipe 3, interchanger 4 and recycle pump 5, injector 2 is arranged on the top of reactor 1, the lower part outlet of reactor 1 is connected by the import of pipeline with recycle pump 5, the outlet of recycle pump 5 is connected by the import of pipeline with interchanger 4, the outlet of interchanger 4 is connected by the top entry of pipeline with injector 2, the side of injector 2 is provided with inlet pipe 3, and inlet pipe 3 is provided with air intake valve.Injector 2 is the venturi-type eductors of jetting type.Interchanger 4 is jacketed still formula interchanger.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in acetonitrile is made into the liquid phase material that mass concentration is 40%, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control entering from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 10-55 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.02:1, stop logical chlorine, close recycle pump 5, obtain the acetonitrile solution containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure acetonitrile, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product rectification under vacuum, GC normalizing content 99.3%, yield 86%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 2
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, adopt injection circulation reactor, the difference of injection circulation reactor and embodiment 1 is that interchanger 4 is plate-type heat exchanger.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in 1, the liquid phase material that mass concentration is 40% is made in 2-ethylene dichloride, join in reactor 1, ON cycle pump 5, liquid phase material pressurize through recycle pump 5, interchanger 4 heat exchange temperature control entering from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 10-55 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.05:1, stop logical chlorine, close recycle pump 5, obtain 1, the 2-dichloroethane solution containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure 1,2-ethylene dichloride, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product rectification under vacuum, GC normalizing content 99%, yield 79%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 3
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, adopt injection circulation reactor, the difference of injection circulation reactor and embodiment 1 is that interchanger 4 is shell and tube heat exchanger.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in methylene dichloride is made into the liquid phase material that mass concentration is 70%, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control entering from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 20-65 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.1:1, stop logical chlorine, close recycle pump 5, obtain the dichloromethane solution containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure methylene dichloride, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product underpressure distillation, GC normalizing content 98.3%, yield 78%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 4
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, injection circulation reactor is adopted, the same embodiment of injection circulation reactor.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in toluene is made into the liquid phase material that mass concentration is 5%, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control entering from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 0-45 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1:1, stop logical chlorine, close recycle pump 5, obtain the toluene solution containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure toluene, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product underpressure distillation, GC normalizing content 98%, yield 80%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 5
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, adopt injection circulation reactor, injection circulation reactor is with embodiment 2.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in DMF is made into the liquid phase material that mass concentration is 15%, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control entering from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 30-55 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.2:1, stop logical chlorine, close recycle pump 5, obtain the DMF solution containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure DMF, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product rectification under vacuum, GC normalizing content 98.6%, yield 81%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 6
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, adopt injection circulation reactor, injection circulation reactor is with embodiment 2.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in chlorobenzene is made into the liquid phase material that mass concentration is 25%, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control entering from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 10-30 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.15:1, stop logical chlorine, close recycle pump 5, obtain the chlorobenzene solution containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure chlorobenzene, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product rectification under vacuum, GC normalizing content 98%, yield 78%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 7
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, adopt injection circulation reactor, injection circulation reactor is with embodiment 3.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in trichloromethane is made into the liquid phase material that mass concentration is 55%, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control and after enter from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 20-40 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.08:1, stop logical chlorine, close recycle pump 5, obtain the chloroform soln containing 2-chloro-5-chloromethyl thiazole.
Three, obtain 2-chloro-5-chloromethyl thiazole crude product through aftertreatment removed under reduced pressure trichloromethane, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product rectification under vacuum, GC normalizing content 98.7%, yield 79%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).
Embodiment 8
Utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, comprise the following steps:
One, adopt injection circulation reactor, injection circulation reactor is with embodiment 3.
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in trichloromethane and 1, the liquid phase material that mass concentration is 50% is made in 2-ethylene dichloride, join in reactor 1, ON cycle pump 5, liquid phase material pressurizes through recycle pump 5, interchanger 4 heat exchange temperature control and after enter from the top entry of injector 2; Open air intake valve, gaseous state chlorine enters injector 2 through inlet pipe 3 to carry out mixing and reacting with liquid phase material, mixing the top entry of injector 2 got back to by reacted material after reactor 1, recycle pump 5, interchanger 4, circulating reaction, according to the mass fraction fed intake of 1-isothiocyanic acid base-2-chloro-2-propene, calculate the ventilation total amount of chlorine, temperature of reaction 55-65 DEG C; When chlorine total mole number: when the mole number of 1-isothiocyanic acid base-2-chloro-2-propene reaches 1.12:1, stop logical chlorine, close recycle pump 5, obtain the trichloromethane containing 2-chloro-5-chloromethyl thiazole and 1,2-ethylene dichloride mixing solutions.
Three, through aftertreatment removed under reduced pressure trichloromethane and 1,2-ethylene dichloride obtains 2-chloro-5-chloromethyl thiazole crude product, obtain qualified 2-chloro-5-chloromethyl thiazole product after crude product rectification under vacuum, GC normalizing content 98.6%, yield 82%(calculates with 1-isothiocyanic acid base-2-chloro-2-propene).

Claims (10)

1. utilize injection circulation reactor to prepare a method for 2-chloro-5-chloromethyl thiazole, it is characterized in that, comprise the following steps:
One, adopt injection circulation reactor, described injection circulation reactor comprises reactor (1), injector (2), inlet pipe (3), interchanger (4) and recycle pump (5), described injector (2) is arranged on the top of reactor (1), the lower part outlet of reactor (1) is connected by the import of pipeline with recycle pump (5), the outlet of recycle pump (5) is connected by the import of pipeline with interchanger (4), the outlet of interchanger (4) is connected by the top entry of pipeline with injector (2), the side of injector (2) is provided with inlet pipe (3), inlet pipe (3) is provided with air intake valve,
Two, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in inert organic solvents is made into liquid phase material, join in reactor (1), ON cycle pump (5), liquid phase material is through recycle pump (5) pressurization, interchanger (4) heat exchange temperature control entering from the top entry of injector (2); Open air intake valve, gaseous state chlorine enters injector (2) through inlet pipe (3) to carry out mixing and reacting with liquid phase material, mixing the top entry of injector (2) got back to by reacted material after reactor (1), recycle pump (5), interchanger (4), chlorine passes in proportion, after circulating reaction to logical chlorine terminates, obtain the solution containing 2-chloro-5-chloromethyl thiazole;
Three, through aftertreatment precipitation, refining after obtain qualified 2-chloro-5-chloromethyl thiazole product.
2. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 1, is characterized in that, the venturi-type eductors that injector (2) is jetting type.
3. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 1, it is characterized in that, interchanger (4) is the combination of one or two or more kinds in jacketed still formula interchanger, plate-type heat exchanger or shell and tube heat exchanger.
4. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 1, is characterized in that, 1-isothiocyanic acid base-2-chloro-2-propene is dissolved in inert organic solvents and is made into the liquid phase material that mass concentration is 5% ~ 70%.
5. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 1, is characterized in that, temperature of reaction is 0-65 DEG C.
6. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 5, is characterized in that, temperature of reaction is 10-55 DEG C.
7. utilize injection circulation reactor to prepare the method for 2-chloro-5-chloromethyl thiazole according to claim 1, it is characterized in that, described ratio is: the final mol ratio of 1-isothiocyanic acid base-2-chloro-2-propene and chlorine is 1:1-1.2.
8. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 7, is characterized in that, the final mol ratio of 1-isothiocyanic acid base-2-chloro-2-propene and chlorine is 1:1-1.1.
9. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 1, it is characterized in that, inert organic solvents is selected from toluene, acetonitrile, DMF, chlorobenzene, 1,2-ethylene dichloride, trichloromethane, the mixture of one or two or more kinds in methylene dichloride.
10. the method utilizing injection circulation reactor to prepare 2-chloro-5-chloromethyl thiazole according to claim 1, it is characterized in that, aftertreatment precipitation is removed under reduced pressure inert organic solvents, refines as rectification under vacuum or underpressure distillation.
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CN109293596A (en) * 2018-09-30 2019-02-01 江苏润泽鑫生物科技有限公司 The preparation method of 2- chloro-5-chloromethyl thiazole
CN109293512A (en) * 2018-12-10 2019-02-01 杭州若水化学科技有限公司 Esters of acrylic acid product production device
CN109369469A (en) * 2018-11-29 2019-02-22 浙江秦燕科技股份有限公司 The method of successive reaction preparation CLT acid chloride
CN109593053A (en) * 2018-11-29 2019-04-09 浙江秦燕科技股份有限公司 The method of successive reaction preparation CLT acid itrated compound
CN109810024A (en) * 2019-03-28 2019-05-28 南京工业大学 A kind of spray circuits reactor being used to prepare penta diisocyanate and its application method
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CN110511142A (en) * 2019-08-29 2019-11-29 青岛科技大学 A kind of continuous production system and production technology of methylvinyl acetate
CN112429743A (en) * 2021-01-04 2021-03-02 岳阳明科催化技术有限公司 Carbonization device and method for producing ultrafine white carbon black by carbonization method
CN112551565A (en) * 2021-01-07 2021-03-26 岳阳明科催化技术有限公司 Carbonizing device and method for producing macroporous pseudo-boehmite by carbonization method
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CN117466810A (en) * 2023-12-26 2024-01-30 北京弗莱明科技有限公司 Industrial continuous production method of picloram

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CN107537405A (en) * 2016-06-26 2018-01-05 江苏托球农化股份有限公司 A kind of logical chlorine device
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CN109369469A (en) * 2018-11-29 2019-02-22 浙江秦燕科技股份有限公司 The method of successive reaction preparation CLT acid chloride
CN109593053A (en) * 2018-11-29 2019-04-09 浙江秦燕科技股份有限公司 The method of successive reaction preparation CLT acid itrated compound
CN109293512A (en) * 2018-12-10 2019-02-01 杭州若水化学科技有限公司 Esters of acrylic acid product production device
CN109810024A (en) * 2019-03-28 2019-05-28 南京工业大学 A kind of spray circuits reactor being used to prepare penta diisocyanate and its application method
CN110252211A (en) * 2019-07-15 2019-09-20 宁夏贝利特生物科技有限公司 The method of 2- chloro-5-chloromethyl thiazole is continuously synthesized in a kind of tube type falling-film reactor
CN110511142A (en) * 2019-08-29 2019-11-29 青岛科技大学 A kind of continuous production system and production technology of methylvinyl acetate
CN112429743A (en) * 2021-01-04 2021-03-02 岳阳明科催化技术有限公司 Carbonization device and method for producing ultrafine white carbon black by carbonization method
CN112551565A (en) * 2021-01-07 2021-03-26 岳阳明科催化技术有限公司 Carbonizing device and method for producing macroporous pseudo-boehmite by carbonization method
CN115109008A (en) * 2022-07-05 2022-09-27 山西玉龙化工有限公司 Method for prolonging reuse of toluene solvent in preparation of 2-chloro-5-chloromethyl thiazole
CN115109008B (en) * 2022-07-05 2024-02-06 山西玉龙化工有限公司 Method for prolonging toluene solvent application in preparation of 2-chloro-5-chloromethylthiazole
CN117466810A (en) * 2023-12-26 2024-01-30 北京弗莱明科技有限公司 Industrial continuous production method of picloram

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