CN211284207U - 2-chlorine-3-trifluoromethyl pyridine synthesizer - Google Patents
2-chlorine-3-trifluoromethyl pyridine synthesizer Download PDFInfo
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- CN211284207U CN211284207U CN201922327866.4U CN201922327866U CN211284207U CN 211284207 U CN211284207 U CN 211284207U CN 201922327866 U CN201922327866 U CN 201922327866U CN 211284207 U CN211284207 U CN 211284207U
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Abstract
The utility model relates to a 2-chlorine-3-trifluoromethylpyridine synthesizer, synthesizer is including the multistage chlorination cauldron, first rectifier unit, crystallization kettle, fluorination cauldron, neutralization cauldron, the second rectifier unit that communicate the setting in proper order. The synthesis device of the 2-chloro-3-trifluoromethylpyridine of the utility model can utilize the chlorine gas with the highest efficiency through the arrangement of the multistage chlorination kettles which are communicated in sequence, thereby avoiding the waste of the chlorine gas, simultaneously leading the reaction to be more complete and improving the yield of reaction products; the high-purity end product 2-chloro-3-trifluoromethylpyridine can be safely and efficiently obtained by sequentially passing through the first rectifying device, the crystallizing kettle, the fluorinating kettle, the neutralizing kettle and the second rectifying device. Utilize synthesizer's synthetic route is simple high-efficient, and gained product purity is high, promotes the production security by a wide margin, easily industrialization popularization.
Description
Technical Field
The utility model relates to a chemical synthesis technical field, concretely relates to 2-chlorine-3-trifluoromethyl pyridine synthesizer.
Background
The 2-chloro-3-trifluoromethylpyridine is a novel pesticide intermediate, has wide application in the fields of organic synthetic dyes, medicines and the like, and is also a key intermediate for synthesizing a high-efficiency low-toxicity herbicide pyrazosulfuron-ethyl.
In the prior art, 2-chloro-3-trifluoromethylpyridine is generally used as a raw material to synthesize the 2-chloro-3-trifluoromethylpyridine in the presence of a catalyst, and the synthesis route is roughly two: 1) performing chlorofluorination in a reactor to synthesize 2-chloro-3-trifluoromethylpyridine in one step; 2) the step-by-step method comprises the steps of firstly chlorinating and then fluorinating to synthesize the 2-chloro-3-trifluoromethylpyridine, wherein the reaction for synthesizing the 2-chloro-3-trifluoromethylpyridine by the two common synthesis methods in the prior art is generally carried out under the catalytic action of a catalyst. However, the catalyst used is either expensive (such as manganese fluoride, etc.), not readily available (such as cobalt chloride, etc.), or unsafe, very explosive (such as azo); the existing synthesis equipment of 2-chloro-3-trifluoromethylpyridine wastes chlorine seriously, so that the industrial synthesis production cost is increased, and serious potential safety hazard exists.
SUMMERY OF THE UTILITY MODEL
The technical problem to be solved by the utility model is that the synthetic process of 2-chloro-3-trifluoromethyl pyridine in the prior art needs to use the catalyst which is easy to explode, expensive or not easy to obtain and the waste of chlorine is serious and the like. 2-chlorine-3-trifluoromethylpyridine's synthesizer can realize the demand that can prepare high-purity 2-chlorine-3-trifluoromethylpyridine product without the catalyst, and the synthetic route is simple high-efficient, and the raw materials is with low costs, and gained product purity is high, promotes the production security by a wide margin, easily industrialization popularization.
In order to solve the technical problem, the utility model discloses a technical scheme as follows:
a2-chloro-3-trifluoromethylpyridine synthesis device comprises a multistage chlorination kettle, a first rectification device, a crystallization kettle, a fluorination kettle, a neutralization kettle and a second rectification device which are sequentially communicated; the multistage chlorination kettle comprises more than two stages of chlorination kettles.
The multistage chlorination kettle comprises a first-stage chlorination kettle, a second-stage chlorination kettle and a third-stage chlorination kettle;
the upper end of the third-stage chlorination kettle is provided with a first feeding hole, and the lower end of the third-stage chlorination kettle is provided with a first discharging hole;
the upper end of the secondary chlorination kettle is provided with a second feeding hole and a first discharging hole, and the lower end of the secondary chlorination kettle is provided with a second discharging hole;
the upper end of the primary chlorination kettle is provided with a third feeding hole, a second material pouring hole and a chlorine introducing hole, and the lower end of the primary chlorination kettle is provided with a third discharging hole;
a first chlorine channel is arranged between the third-stage chlorination kettle and the second-stage chlorination kettle, and a second chlorine channel is arranged between the second-stage chlorination kettle and the first-stage chlorination kettle;
the first discharge port is communicated with the first material pouring port, and the second discharge port is communicated with the second material pouring port.
Further, the first rectifying device is provided with a fourth feeding hole and a fourth discharging hole; and the fourth feeding hole is communicated with the third discharging hole.
Further, the crystallization kettle is provided with a fifth feeding hole and a fifth discharging hole; and the fifth feeding hole is communicated with the fourth discharging hole.
Further, the fluorination kettle is provided with a hydrogen fluoride inlet, a sixth discharge hole and a sixth feed inlet; and the sixth feeding hole is communicated with the fifth discharging hole.
Further, the neutralization kettle is provided with a water inlet, a seventh discharge hole, a seventh feed inlet and an alkali inlet; and the seventh feeding hole is communicated with the sixth discharging hole.
Further, the second rectifying device is provided with an eighth feeding hole and a finished product discharging hole; and the eighth feeding hole is communicated with the seventh discharging hole.
Further, stirring devices are arranged in the third-stage chlorination kettle, the second-stage chlorination kettle, the first-stage chlorination kettle, the crystallization kettle, the fluorination kettle and the neutralization kettle.
Furthermore, a return pipeline is arranged between the primary chlorination kettle and the first rectifying device.
Further, the tertiary chlorination cauldron, crystallization kettle and fluorination cauldron all are provided with tail gas absorbing device.
Further, the second rectifying device is provided with a reaction byproduct collecting device.
A preparation method of 2-chloro-3-trifluoromethylpyridine comprises the following steps:
(1) dissolving 2-chloro-3-methylpyridine in an organic solvent, introducing chlorine gas for reaction to obtain a chlorinated crude product, performing reduced pressure rectification and crystallization on the chlorinated crude product, and separating to obtain 2-chloro-3-trichloromethylpyridine;
(2) introducing hydrogen fluoride into the 2-chloro-3-trichloromethylpyridine for reaction to obtain a reaction product, adding water and alkali into the reaction product for reaction, and standing for layering to obtain a crude fluorinated product;
(3) and carrying out separation and purification treatment on the crude fluorination product to obtain a separated and purified product, and carrying out reduced pressure rectification on the separated and purified product to obtain the 2-chloro-3-trifluoromethylpyridine.
Further, in the step (1), the organic solvent is any one of chlorobenzene, carbon tetrachloride, dichlorobenzene or o-dichlorobenzene.
Further, in the step (1), the molar ratio of the 2-chloro-3-trifluoromethylpyridine to the organic solvent is 1 (2-10).
Further, in the step (1), the speed of introducing the chlorine is 38-42kg/h, and the chlorination reaction is a multistage chlorination process; the reaction temperature is 100-160 ℃, the reaction time is 10-12h, and the reaction pressure is normal pressure.
Further, the multistage chlorination process is any one of a two-stage chlorination process, a three-stage chlorination process and a four-stage chlorination process.
Further, the tertiary chlorination process comprises the following steps: dividing 2-chloro-3-methylpyridine dissolved in an organic solvent into three equal parts, respectively putting the three equal parts into three reaction kettles, allowing chlorine to pass through the three reaction kettles in sequence, and taking out a chlorinated crude product from a first-stage reaction kettle for rectification after the reaction is finished; introducing the chlorinated crude product in the second-stage reaction kettle into the first-stage reaction kettle, introducing the chlorinated crude product in the third-stage reaction kettle into the second-stage reaction kettle, adding new 2-chloro-3-methylpyridine dissolved in the organic solvent into the third-stage reaction kettle again, and continuously introducing chlorine gas for continuous reaction; through tertiary chlorination process, can effectively practice thrift the chlorine use amount, and can make the reaction more abundant complete simultaneously, improve the yield of reaction product.
Further, in the step (1), the pressure of the reduced pressure distillation is between-0.08 MPa and-0.02 MPa, and the fraction at 140 ℃ and 160 ℃ in the reduced pressure distillation is the 2-chloro-3-trichloromethylpyridine.
Further, in the step (2), when the hydrogen fluoride is introduced, the temperature of the 2-chloro-3-trichloromethyl pyridine is 78-82 ℃.
Further, in the step (2), the molar ratio of the 2-chloro-3-trichloromethylpyridine to the hydrogen fluoride is 1 (7-20).
Further, in the step (2), the temperature for introducing the hydrogen fluoride to carry out the reaction is 160-210 ℃, the reaction time is 8-12h, and the reaction pressure is 3-9 MPa.
Further, in the step (2), the adding amount of the water is 90-110% of the mass of the reaction product; and adding alkali to adjust the pH value of the system to 6.9-7.1, wherein the alkali is any one of sodium hydroxide or potassium hydroxide. The main purpose of adding water and alkali is to remove hydrogen fluoride and hydrogen chloride from the reaction system.
Further, in the step (3), the separation and purification treatment method is any one of centrifugation, crystallization or filter pressing; the temperature of the circulating water of the reduced pressure distillation is 35-40 ℃, the pressure of the reduced pressure distillation is-0.99 MPa to-0.08 MPa, and the fraction with the temperature of 100 ℃ and 150 ℃ in the reduced pressure distillation is the 2-chloro-3-trifluoromethylpyridine.
Compared with the prior art, the technical scheme of the utility model have following advantage:
the synthesis device of the 2-chloro-3-trifluoromethylpyridine of the utility model can utilize the chlorine gas with the highest efficiency through the arrangement of the multistage chlorination kettles which are communicated in sequence, thereby avoiding the waste of the chlorine gas, simultaneously leading the reaction to be more complete and improving the yield of reaction products; the purity of the intermediate reaction product 2-chloro-3-trichloromethylpyridine can be greatly improved through the first rectifying device, so that the fluorination reaction can be effectively carried out, and the product yield is indirectly improved; the purity of the intermediate product 2-chloro-3-trichloromethylpyridine can be further improved through the crystallization kettle; 2-chloro-3-trichloromethyl pyridine can be efficiently fluorinated through the fluorination kettle, hydrogen fluoride is fully utilized, and the synthesis cost is further reduced; and finally, the final product 2-chloro-3-trifluoromethylpyridine can be efficiently purified through the neutralization kettle and the second rectifying device, and finally, a high-purity product is safely and efficiently obtained.
Synthesizer can effectively guarantee going on smoothly of reaction to the security of synthetic process has effectively been promoted. The purity of the 2-chloro-3-trifluoromethyl pyridine prepared by the synthesis equipment of the utility model is more than 99 percent, and the yield is more than 80 percent.
The synthesis equipment of the utility model can meet the requirement of preparing high-purity 2-chloro-3-trifluoromethylpyridine products without using catalysts, thereby reducing the synthesis cost and greatly improving the production safety; utilize the simple high efficiency of synthesis process of synthesizer, the raw materials cost is low, and gained product purity is high, guarantees the production security, easily industrialization popularization.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of a 2-chloro-3-trifluoromethylpyridine synthesis apparatus according to example 1 of the present invention;
in the figure, 1-a third-stage chlorination kettle; 110-a first feed port; 120-a first discharge port; 2-a secondary chlorination kettle; 21-a second feed port; 22-a second discharge port; 23-a first material pouring port; 3-a first-stage chlorination kettle; 31-a third feed port; 32-a third discharge hole; 33-a second material pouring port; 34-a chlorine gas inlet; 4-a first rectification device; 41-a fourth feed port; 42-a fourth discharge hole; 5-crystallization kettle; 51-a fifth feed port; 52-fifth discharge port; 6-fluorination kettle; 61-a hydrogen fluoride inlet; 62-a sixth discharge port; 63-sixth feed inlet; 7-a neutralization kettle; 71-a water inlet; 72-seventh discharge port; 73-a seventh feed port; 74-an alkali introduction port; 8-a second rectification unit; 81-eighth feed inlet; 82-finished product discharge hole; 9-a first chlorine channel; 10-a second chlorine channel; 11-a stirring device; 12-a return line;
FIG. 2 is a diagram of an apparatus for tertiary chlorination according to embodiment 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the technical solutions of the present invention will be described in detail below. It is to be understood that the embodiments described are only some embodiments of the invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by a person skilled in the art without creative efforts belong to the protection scope of the present invention.
Example 1
The embodiment provides a synthesis device of 2-chloro-3-trifluoromethylpyridine, as shown in fig. 1 and fig. 2, comprising a three-stage chlorination kettle 1, a two-stage chlorination kettle 2, a one-stage chlorination kettle 3, a first rectification device 4, a crystallization kettle 5, a fluorination kettle 6, a neutralization kettle 7, and a second rectification device 8, which are sequentially communicated; the upper end of the three-stage chlorination kettle 1 is provided with a first feeding hole 110, and the lower end is provided with a first discharging hole 120; the upper end of the secondary chlorination kettle 2 is provided with a second feeding hole 21 and a first discharging hole 23, and the lower end is provided with a second discharging hole 22; the upper end of the first-stage chlorination kettle 3 is provided with a third feeding port 31, a second material pouring port 33 and a chlorine introducing port 34, and the lower end is provided with a third discharging port 32; a first chlorine channel 9 is arranged between the third-stage chlorination kettle 1 and the second-stage chlorination kettle 2, and a second chlorine channel 10 is arranged between the second-stage chlorination kettle 2 and the first-stage chlorination kettle 3;
the first rectifying device 4 is provided with a fourth feeding hole 41 and a fourth discharging hole 42, and the fourth feeding hole 41 is communicated with the third discharging hole 32; the crystallization kettle 5 is provided with a fifth feed inlet 51 and a fifth discharge outlet 52, and the fifth feed inlet 51 is communicated with the fourth discharge outlet 42; the fluorination kettle is provided with a hydrogen fluoride inlet 61, a sixth discharge hole 62 and a sixth feed inlet 63, and the sixth feed inlet 63 is communicated with the fifth discharge hole 52; the neutralization kettle 7 is provided with a water inlet 71, a seventh discharge hole 72, a seventh feed inlet 73 and an alkali inlet 74, and the seventh feed inlet 73 is communicated with the sixth discharge hole 62; the second rectifying device 8 is provided with an eighth feeding hole 81 and a finished product discharging hole 82, and the eighth feeding hole 81 is communicated with the seventh discharging hole 72.
The embodiment provides a preparation method of 2-chloro-3-trifluoromethylpyridine, and the specific treatment method comprises the following steps:
(1) dissolving 1000g of 2-chloro-3-methylpyridine with the purity of 99% by 1731g of chlorobenzene, then averagely dividing into three parts, respectively putting the three parts into a third-stage chlorination kettle 1, a second-stage chlorination kettle 2 and a first-stage chlorination kettle 3 through a first feed inlet 110, a second feed inlet 21 and a third feed inlet 31, adjusting the reaction temperature to 100 ℃, introducing chlorine gas into the first-stage reaction kettle 3 from a chlorine gas introduction port 34 at the speed of 38-42kg/h, respectively introducing the chlorine gas into the second-stage reaction kettle 2 and the third-stage reaction kettle 1 through a first chlorine gas channel 9 and a second chlorine gas channel 10, continuously introducing the chlorine gas, keeping the chlorine gas for 10 hours, and performing chlorination reaction to obtain a chlorinated crude product; putting the chlorinated crude product in the first-stage reaction kettle 3 into a first rectifying device 4 through a third discharge hole 32 and a fourth feed hole 41 for rectification under reduced pressure, introducing the chlorinated crude product obtained in the second-stage reaction kettle 2 into the first-stage reaction kettle 3, introducing the chlorinated crude product obtained in the third-stage reaction kettle 1 into the second-stage reaction kettle 2, adding new 2-chloro-3-methylpyridine dissolved in an organic solvent into the third-stage reaction kettle 1 again, and continuously introducing chlorine for continuous reaction; the pressure of the reduced pressure distillation in the first distillation device 4 is controlled to be-0.02 MPa, fractions at 150 ℃ are collected, the fractions enter a crystallization kettle 5 through a fourth discharge hole 42 and a fifth feed hole 51 for crystallization, the crystals are collected, 1580.6g of 2-chloro-3-trichloromethylpyridine is obtained, the yield is 88.7%, the content is 94.9%, and the reaction liquid after the reduced pressure distillation flows back to the first-stage reaction kettle through a reflux pipeline 12 for continuous reaction.
(2) Keeping the temperature of the fluorination kettle 6 at 80 ℃, putting the 2-chloro-3-trichloromethylpyridine into the fluorination kettle 6 through a fifth discharge hole 52 and a sixth feed hole 63, after the feeding is finished, increasing the temperature of the fluorination kettle 6 to 160 ℃, keeping the pressure at 3MPa, introducing 981g of hydrogen fluoride from a hydrogen fluoride introduction hole 61, and reacting for 8 hours to obtain a reaction product; after the reaction is finished, cooling, slowly discharging pressure for 3 hours, expelling acid gas by using nitrogen, pressing materials by using nitrogen, and reducing the reaction pressure to normal pressure; and (3) putting the reaction product into a neutralization kettle 7 through a sixth discharge hole 62 and a seventh feed hole 73, adding water accounting for 90% of the mass of the reaction product into the reaction product through a water inlet 71, adding sodium hydroxide through an alkali inlet 74 to adjust the pH of the reaction system to 6.9, removing hydrogen fluoride and hydrogen chloride, and standing for layering to obtain a crude fluorinated product.
(3) Putting the fluorinated crude product into a second rectifying device 8 through a seventh discharge hole 72 and an eighth feed hole 81, and firstly, carrying out filter pressing treatment on the fluorinated crude product to obtain a separated and purified product; then, carrying out reduced pressure rectification on the separated and purified product, wherein the pressure of the reduced pressure rectification is kept at-0.08 Mpa, and the water temperature of circulating water of a condenser is 35 ℃; and collecting fractions at 100 ℃, finally collecting 824.2g of 2-chloro-3-trifluoromethylpyridine from a finished product discharge port 82, and analyzing by gas chromatography, wherein the yield is 81.3 percent and the content is 99 percent.
Example 2
The embodiment provides a synthesis device of 2-chloro-3-trifluoromethylpyridine, which comprises a third chlorination kettle 1, a second chlorination kettle 2, a first chlorination kettle 3, a first rectification device 4, a crystallization kettle 5, a fluorination kettle 6, a neutralization kettle 7 and a second rectification device 8 which are sequentially communicated; the upper end of the three-stage chlorination kettle 1 is provided with a first feeding hole 110, and the lower end is provided with a first discharging hole 120; the upper end of the secondary chlorination kettle 2 is provided with a second feeding hole 21 and a first discharging hole 23, and the lower end is provided with a second discharging hole 22; the upper end of the first-stage chlorination kettle 3 is provided with a third feeding port 31, a second material pouring port 33 and a chlorine introducing port 34, and the lower end is provided with a third discharging port 32; a first chlorine channel 9 is arranged between the third-stage chlorination kettle 1 and the second-stage chlorination kettle 2, and a second chlorine channel 10 is arranged between the second-stage chlorination kettle 2 and the first-stage chlorination kettle 3;
the first rectifying device 4 is provided with a fourth feeding hole 41 and a fourth discharging hole 42, and the fourth feeding hole 41 is communicated with the third discharging hole 32; the crystallization kettle 5 is provided with a fifth feed inlet 51 and a fifth discharge outlet 52, and the fifth feed inlet 51 is communicated with the fourth discharge outlet 42; the fluorination kettle is provided with a hydrogen fluoride inlet 61, a sixth discharge hole 62 and a sixth feed inlet 63, and the sixth feed inlet 63 is communicated with the fifth discharge hole 52; the neutralization kettle 7 is provided with a water inlet 71, a seventh discharge hole 72, a seventh feed inlet 73 and an alkali inlet 74, and the seventh feed inlet 73 is communicated with the sixth discharge hole 62; the second rectifying device 8 is provided with an eighth feeding hole 81 and a finished product discharging hole 82, and the eighth feeding hole 81 is communicated with the seventh discharging hole 72; the three-stage chlorination kettle 1, the two-stage chlorination kettle 2, the one-stage chlorination kettle 3, the crystallization kettle 5, the fluorination kettle 6 and the neutralization kettle 7 all contain stirring devices 11; a return pipeline 12 is arranged between the primary chlorination kettle 3 and the first rectifying device 4; the three-stage chlorination kettle 1, the crystallization kettle 5 and the fluorination kettle 6 are all provided with tail gas absorption devices; the second rectifying device 8 is provided with a reaction byproduct collecting device.
The embodiment provides a preparation method of 2-chloro-3-trifluoromethylpyridine, and the specific treatment method comprises the following steps:
(1) dissolving 1000g of 99% pure 2-chloro-3-methylpyridine by 3463g of dichlorobenzene, evenly dividing into three parts, respectively putting the three parts into a third-stage chlorination kettle 1, a second-stage chlorination kettle 2 and a first-stage chlorination kettle 3 at a first feed inlet 110, a second feed inlet 21 and a third feed inlet 31, adjusting the reaction temperature to 115 ℃, introducing chlorine gas into the first-stage chlorination kettle 3 from a chlorine gas introduction port 34 at a speed of 42kg/h, respectively introducing the chlorine gas into the second-stage reaction kettle 2 and the third-stage reaction kettle 1 through a first chlorine gas channel 9 and a second chlorine gas channel 10, continuously introducing the chlorine gas, keeping the chlorine gas for 10.5 hours, and performing chlorination reaction to obtain a chlorinated crude product; putting the chlorinated crude product in the first-stage reaction kettle 3 into a first rectifying device 4 through a third discharge hole 32 and a fourth feed hole 41 for rectification under reduced pressure, introducing the chlorinated crude product obtained in the second-stage reaction kettle 2 into the first-stage reaction kettle 3, introducing the chlorinated crude product obtained in the third-stage reaction kettle 1 into the second-stage reaction kettle 2, adding new 2-chloro-3-methylpyridine dissolved in an organic solvent into the third-stage reaction kettle 1 again, and continuously introducing chlorine for continuous reaction; the pressure of the reduced pressure distillation in the first distillation device 4 is controlled to be-0.03 MPa, fractions at 150 ℃ are collected, the fractions enter the crystallization kettle 5 through the fourth discharge hole 42 and the fifth feed hole 51 for crystallization, crystals are collected, 1610.9g of 2-chloro-3-trichloromethylpyridine is obtained, the yield is 90.4%, the content is 95.1%, and the reaction liquid after the reduced pressure distillation flows back to the first-stage reaction kettle through the reflux pipeline 12 for continuous reaction.
(2) Keeping the temperature of the fluorination kettle 6 at 85 ℃, putting the 2-chloro-3-trichloromethylpyridine into the fluorination kettle 6 through a fifth discharge hole 52 and a sixth feed hole 63, after the feeding is finished, increasing the temperature of the fluorination kettle 6 to 170 ℃, keeping the pressure at 3.5MPa, introducing 1428g of hydrogen fluoride from a hydrogen fluoride introduction hole 61, and reacting for 9 hours to obtain a reaction product; after the reaction is finished, cooling, slowly discharging pressure for 4 hours, expelling acid gas by using nitrogen, pressing materials by using nitrogen, and reducing the reaction pressure to normal pressure; and (3) putting the reaction product into a neutralization kettle 7 through a sixth discharge hole 62 and a seventh feed hole 73, adding water accounting for 90% of the mass of the reaction product into the reaction product through a water inlet 71, adding sodium hydroxide through an alkali inlet 74 to adjust the pH of the reaction system to 6.9, removing hydrogen fluoride and hydrogen chloride, and standing for layering to obtain a crude fluorinated product.
(3) Putting the fluorinated crude product into a second rectifying device 8 through a seventh discharge hole 72 and an eighth feed hole 81, and firstly, carrying out crystallization treatment on the fluorinated crude product to obtain a separated and purified product; and then, carrying out reduced pressure rectification on the separated and purified product, wherein the pressure of the reduced pressure rectification is kept at-0.20 Mpa, and the temperature of the circulating water of the condenser is 35 ℃. And collecting 100 ℃ fractions, finally collecting 844.4g of 2-chloro-3-trifluoromethylpyridine from a finished product discharge port 82, and analyzing by gas chromatography, wherein the yield is 83.3 percent and the content is 99.2 percent.
Example 3
The embodiment provides a synthesis device of 2-chloro-3-trifluoromethylpyridine, which comprises a third chlorination kettle 1, a second chlorination kettle 2, a first chlorination kettle 3, a first rectification device 4, a crystallization kettle 5, a fluorination kettle 6, a neutralization kettle 7 and a second rectification device 8 which are sequentially communicated; the upper end of the three-stage chlorination kettle 1 is provided with a first feeding hole 110, and the lower end is provided with a first discharging hole 120; the upper end of the secondary chlorination kettle 2 is provided with a second feeding hole 21 and a first discharging hole 23, and the lower end is provided with a second discharging hole 22; the upper end of the first-stage chlorination kettle 3 is provided with a third feeding port 31, a second material pouring port 33 and a chlorine introducing port 34, and the lower end is provided with a third discharging port 32; a first chlorine channel 9 is arranged between the third-stage chlorination kettle 1 and the second-stage chlorination kettle 2, and a second chlorine channel 10 is arranged between the second-stage chlorination kettle 2 and the first-stage chlorination kettle 3;
the first rectifying device 4 is provided with a fourth feeding hole 41 and a fourth discharging hole 42, and the fourth feeding hole 41 is communicated with the third discharging hole 32; the crystallization kettle 5 is provided with a fifth feed inlet 51 and a fifth discharge outlet 52, and the fifth feed inlet 51 is communicated with the fourth discharge outlet 42; the fluorination kettle is provided with a hydrogen fluoride inlet 61, a sixth discharge hole 62 and a sixth feed inlet 63, and the sixth feed inlet 63 is communicated with the fifth discharge hole 52; the neutralization kettle 7 is provided with a water inlet 71, a seventh discharge hole 72, a seventh feed inlet 73 and an alkali inlet 74, and the seventh feed inlet 73 is communicated with the sixth discharge hole 62; the second rectifying device 8 is provided with an eighth feeding hole 81 and a finished product discharging hole 82, and the eighth feeding hole 81 is communicated with the seventh discharging hole 72; the three-stage chlorination kettle 1, the two-stage chlorination kettle 2, the one-stage chlorination kettle 3, the crystallization kettle 5, the fluorination kettle 6 and the neutralization kettle 7 all contain stirring devices 11; a return pipeline 12 is arranged between the primary chlorination kettle 3 and the first rectifying device 4; the three-stage chlorination kettle 1, the crystallization kettle 5 and the fluorination kettle 6 are all provided with tail gas absorption devices; the second rectifying device 8 is provided with a reaction byproduct collecting device.
The embodiment provides a preparation method of 2-chloro-3-trifluoromethylpyridine, and the specific treatment method comprises the following steps:
(1) dissolving 1000g of 2-chloro-3-methylpyridine with the purity of 99% by using 5194g of carbon tetrachloride, then evenly dividing into three parts, respectively putting the three parts into a third-stage chlorination kettle 1, a second-stage chlorination kettle 2 and a first-stage chlorination kettle 3 through a first feed inlet 110, a second feed inlet 21 and a third feed inlet 31, adjusting the reaction temperature to 130 ℃, introducing chlorine gas into the first-stage reaction kettle 3 from a chlorine gas introduction port 34 at the speed of 39kg/h, respectively introducing the chlorine gas into the second-stage reaction kettle 2 and the third-stage reaction kettle 1 through a first chlorine gas channel 9 and a second chlorine gas channel 10, continuously introducing the chlorine gas, keeping the chlorine gas for 11 hours, and carrying out chlorination reaction to obtain a chlorinated crude product; putting the chlorinated crude product in the first-stage reaction kettle 3 into a first rectifying device 4 through a third discharge hole 32 and a fourth feed hole 41 for rectification under reduced pressure, introducing the chlorinated crude product obtained in the second-stage reaction kettle 2 into the first-stage reaction kettle 3, introducing the chlorinated crude product obtained in the third-stage reaction kettle 1 into the second-stage reaction kettle 2, adding new 2-chloro-3-methylpyridine dissolved in an organic solvent into the third-stage reaction kettle 1 again, and continuously introducing chlorine for continuous reaction; the pressure of the reduced pressure distillation in the first distillation device 4 is controlled to be-0.05 MPa, fractions at 150 ℃ are collected, the fractions enter the crystallization kettle 5 through the fourth discharge hole 42 and the fifth feed hole 51 for crystallization, crystals are collected, 1621.6g of 2-chloro-3-trichloromethylpyridine is obtained, the yield is 91.0%, the content is 96.1%, and the reaction liquid after the reduced pressure distillation flows back to the first-stage reaction kettle through the reflux pipeline 12 for continuous reaction.
(2) Keeping the temperature of the fluorination kettle 6 at 90 ℃, and feeding the 2-chloro-3-trichloromethyl pyridine into the fluorination kettle 6 through a fifth discharge hole 52 and a sixth feed hole 63. After the feeding is finished, the temperature of the fluorination kettle 6 is increased to 185 ℃, the pressure is kept at 4MPa, 2012g of hydrogen fluoride is introduced from the hydrogen fluoride inlet 61, and the reaction is carried out for 10 hours to obtain a reaction product. After the reaction is finished, cooling, slowly discharging pressure for 6.5 hours, expelling acid gas by using nitrogen, pressing by using nitrogen, and reducing the reaction pressure to normal pressure; and (3) putting the reaction product into a neutralization kettle 7 through a sixth discharge hole 62 and a seventh feed hole 73, adding water accounting for 110% of the mass of the reaction product into the reaction product through a water inlet 71, adding sodium hydroxide through an alkali inlet 74 to adjust the pH of the reaction system to 7.1, removing hydrogen fluoride and hydrogen chloride, and standing for layering to obtain a crude fluorinated product.
(3) Putting the fluorinated crude product into a second rectifying device 8 through a seventh discharge hole 72 and an eighth feed hole 81, and firstly, carrying out filter pressing treatment on the fluorinated crude product to obtain a separated and purified product; and then, carrying out reduced pressure rectification on the separated and purified product, wherein the pressure of the reduced pressure rectification is kept at-0.61 Mpa, and the temperature of the circulating water of the condenser is 35 ℃. Collecting 100 ℃ fraction, finally collecting 862.7g of 2-chloro-3, 3-fluoromethylpyridine from a finished product discharge port 82, and analyzing by gas chromatography, wherein the yield is 85.1% and the content is 99.5%.
Example 4
The embodiment provides a synthesis device of 2-chloro-3-trifluoromethylpyridine, which comprises a third chlorination kettle 1, a second chlorination kettle 2, a first chlorination kettle 3, a first rectification device 4, a crystallization kettle 5, a fluorination kettle 6, a neutralization kettle 7 and a second rectification device 8 which are sequentially communicated; the upper end of the three-stage chlorination kettle 1 is provided with a first feeding hole 110, and the lower end is provided with a first discharging hole 120; the upper end of the secondary chlorination kettle 2 is provided with a second feeding hole 21 and a first discharging hole 23, and the lower end is provided with a second discharging hole 22; the upper end of the first-stage chlorination kettle 3 is provided with a third feeding port 31, a second material pouring port 33 and a chlorine introducing port 34, and the lower end is provided with a third discharging port 32; a first chlorine channel 9 is arranged between the third-stage chlorination kettle 1 and the second-stage chlorination kettle 2, and a second chlorine channel 10 is arranged between the second-stage chlorination kettle 2 and the first-stage chlorination kettle 3;
the first rectifying device 4 is provided with a fourth feeding hole 41 and a fourth discharging hole 42, and the fourth feeding hole 41 is communicated with the third discharging hole 32; the crystallization kettle 5 is provided with a fifth feed inlet 51 and a fifth discharge outlet 52, and the fifth feed inlet 51 is communicated with the fourth discharge outlet 42; the fluorination kettle is provided with a hydrogen fluoride inlet 61, a sixth discharge hole 62 and a sixth feed inlet 63, and the sixth feed inlet 63 is communicated with the fifth discharge hole 52; the neutralization kettle 7 is provided with a water inlet 71, a seventh discharge hole 72, a seventh feed inlet 73 and an alkali inlet 74, and the seventh feed inlet 73 is communicated with the sixth discharge hole 62; the second rectifying device 8 is provided with an eighth feeding hole 81 and a finished product discharging hole 82, and the eighth feeding hole 81 is communicated with the seventh discharging hole 72; the three-stage chlorination kettle 1, the two-stage chlorination kettle 2, the one-stage chlorination kettle 3, the crystallization kettle 5, the fluorination kettle 6 and the neutralization kettle 7 all contain stirring devices 11; a return pipeline 12 is arranged between the primary chlorination kettle 3 and the first rectifying device 4; the three-stage chlorination kettle 1, the crystallization kettle 5 and the fluorination kettle 6 are all provided with tail gas absorption devices; the second rectifying device 8 is provided with a reaction byproduct collecting device.
The embodiment provides a preparation method of 2-chloro-3-trifluoromethylpyridine, and the specific treatment method comprises the following steps:
(1) dissolving 1000g of 99% pure 2-chloro-3-methylpyridine by 2126g of o-dichlorobenzene, evenly dividing into three parts, respectively putting the three parts into a third-stage chlorination kettle 1, a second-stage chlorination kettle 2 and a first-stage chlorination kettle 3 at a first feed inlet 110, a second feed inlet 21 and a third feed inlet 31, adjusting the reaction temperature to 130 ℃, introducing chlorine gas into the first-stage chlorination kettle 3 from a chlorine gas introduction port 34 at a speed of 40kg/h, respectively introducing the chlorine gas into the second-stage reaction kettle 2 and the third-stage reaction kettle 1 through a first chlorine gas channel 9 and a second chlorine gas channel 10, continuously introducing the chlorine gas, keeping the chlorine gas for 11 hours, and performing chlorination reaction to obtain a chlorinated crude product; putting the chlorinated crude product in the first-stage reaction kettle 3 into a first rectifying device 4 through a third discharge hole 32 and a fourth feed hole 41 for rectification under reduced pressure, introducing the chlorinated crude product obtained in the second-stage reaction kettle 2 into the first-stage reaction kettle 3, introducing the chlorinated crude product obtained in the third-stage reaction kettle 1 into the second-stage reaction kettle 2, adding new 2-chloro-3-methylpyridine dissolved in an organic solvent into the third-stage reaction kettle 1 again, and continuously introducing chlorine for continuous reaction; the pressure of the reduced pressure distillation in the first distillation device 4 is controlled to be-0.07 MPa, fractions at 150 ℃ are collected, the fractions enter the crystallization kettle 5 through the fourth discharge hole 42 and the fifth feed hole 51 for crystallization, crystals are collected, 1621.6g of 2-chloro-3-trichloromethylpyridine is obtained, the yield is 91.0%, the content is 96.1%, and the reaction liquid after the reduced pressure distillation flows back to the first-stage reaction kettle through the reflux pipeline 12 for continuous reaction.
(2) Keeping the temperature of the fluorination kettle 6 at 95 ℃, putting the 2-chloro-3-trichloromethylpyridine into the fluorination kettle 6 through a fifth discharge hole 52 and a sixth feed hole 63, after the feeding is finished, increasing the temperature of the fluorination kettle 6 to 195 ℃, keeping the pressure at 4.5MPa, introducing 2443g of hydrogen fluoride from a hydrogen fluoride introduction hole 61, and reacting for 11 hours to obtain a reaction product; after the reaction is finished, cooling, slowly discharging pressure for 8 hours, expelling acid gas by using nitrogen, pressing materials by using nitrogen, and reducing the reaction pressure to normal pressure; and (3) putting the reaction product into a neutralization kettle 7 through a sixth discharge hole 62 and a seventh feed hole 73, adding water with the same mass into the reaction product through a water introducing port 71, adding sodium hydroxide through an alkali introducing port 74 to adjust the pH value of the reaction system to 7, removing hydrogen fluoride and hydrogen chloride, and standing and layering to obtain a crude fluoride product.
(3) Putting the fluorinated crude product into a second rectifying device 8 through a seventh discharge hole 72 and an eighth feed hole 81, and firstly, carrying out centrifugal treatment on the fluorinated crude product to obtain a separated and purified product; and then, carrying out reduced pressure rectification on the separated and purified product, wherein the vacuum degree needs to be kept at-0.72 Mpa, and the water temperature of the circulating water of the condenser is 35 ℃. And collecting 100 ℃ fractions, and finally collecting 856.6g of 2-chloro-3-trifluoromethylpyridine from a finished product discharge hole 82, wherein the yield is 84.5% and the content is 99.4% by gas chromatography analysis.
Example 5
The embodiment provides a synthesis device of 2-chloro-3-trifluoromethylpyridine, which comprises a third chlorination kettle 1, a second chlorination kettle 2, a first chlorination kettle 3, a first rectification device 4, a crystallization kettle 5, a fluorination kettle 6, a neutralization kettle 7 and a second rectification device 8 which are sequentially communicated; the upper end of the three-stage chlorination kettle 1 is provided with a first feeding hole 110, and the lower end is provided with a first discharging hole 120; the upper end of the secondary chlorination kettle 2 is provided with a second feeding hole 21 and a first discharging hole 23, and the lower end is provided with a second discharging hole 22; the upper end of the first-stage chlorination kettle 3 is provided with a third feeding port 31, a second material pouring port 33 and a chlorine introducing port 34, and the lower end is provided with a third discharging port 32; a first chlorine channel 9 is arranged between the third-stage chlorination kettle 1 and the second-stage chlorination kettle 2, and a second chlorine channel 10 is arranged between the second-stage chlorination kettle 2 and the first-stage chlorination kettle 3;
the first rectifying device 4 is provided with a fourth feeding hole 41 and a fourth discharging hole 42, and the fourth feeding hole 41 is communicated with the third discharging hole 32; the crystallization kettle 5 is provided with a fifth feed inlet 51 and a fifth discharge outlet 52, and the fifth feed inlet 51 is communicated with the fourth discharge outlet 42; the fluorination kettle is provided with a hydrogen fluoride inlet 61, a sixth discharge hole 62 and a sixth feed inlet 63, and the sixth feed inlet 63 is communicated with the fifth discharge hole 52; the neutralization kettle 7 is provided with a water inlet 71, a seventh discharge hole 72, a seventh feed inlet 73 and an alkali inlet 74, and the seventh feed inlet 73 is communicated with the sixth discharge hole 62; the second rectifying device 8 is provided with an eighth feeding hole 81 and a finished product discharging hole 82, and the eighth feeding hole 81 is communicated with the seventh discharging hole 72; the three-stage chlorination kettle 1, the two-stage chlorination kettle 2, the one-stage chlorination kettle 3, the crystallization kettle 5, the fluorination kettle 6 and the neutralization kettle 7 all contain stirring devices 11; a return pipeline 12 is arranged between the primary chlorination kettle 3 and the first rectifying device 4; the three-stage chlorination kettle 1, the crystallization kettle 5 and the fluorination kettle 6 are all provided with tail gas absorption devices; the second rectifying device 8 is provided with a reaction byproduct collecting device.
The embodiment provides a preparation method of 2-chloro-3-trifluoromethylpyridine, and the specific treatment method comprises the following steps:
(1) dissolving 1000g of 99% pure 2-chloro-3-methylpyridine by using 8657g of chlorobenzene, evenly dividing into three parts, respectively putting the three parts into a third-stage chlorination kettle 1, a second-stage chlorination kettle 2 and a first-stage chlorination kettle 3 from a first feed inlet 110, a second feed inlet 21 and a third feed inlet 31, respectively adding 2885g of chlorobenzene from the first feed inlet 110, the second feed inlet 21 and the third feed inlet 31, adjusting the reaction temperature to 130 ℃, introducing chlorine gas into the first-stage reaction kettle 3 from a chlorine gas introduction port 34 at a speed of 41kg/h, respectively introducing the chlorine gas into the second-stage reaction kettle 2 and the third-stage reaction kettle 1 through a first chlorine gas channel 9 and a second chlorine gas channel 10, continuously introducing the chlorine gas, keeping the chlorine gas for 11 hours, and carrying out a third-stage chlorination reaction to obtain a chlorinated crude product; putting the chlorinated crude product in the first-stage reaction kettle 3 into a first rectifying device 4 through a third discharge hole 32 and a fourth feed hole 41 for rectification under reduced pressure, introducing the chlorinated crude product obtained in the second-stage reaction kettle 2 into the first-stage reaction kettle 3, introducing the chlorinated crude product obtained in the third-stage reaction kettle 1 into the second-stage reaction kettle 2, adding new 2-chloro-3-methylpyridine dissolved in an organic solvent into the third-stage reaction kettle 1 again, and continuously introducing chlorine for continuous reaction; the pressure of the reduced pressure distillation in the first distillation device 4 is controlled to be-0.08 MPa, fractions at 150 ℃ are collected, the fractions enter the crystallization kettle 5 through the fourth discharge hole 42 and the fifth feed hole 51 for crystallization, the crystals are collected, 1594.9g of 2-chloro-3-trichloromethylpyridine is obtained, the yield is 89.5%, the content is 94.5%, the content is 94.9%, and the reaction liquid after the reduced pressure distillation flows back to the first-stage reaction kettle through the reflux pipeline 12 for continuous reaction.
(2) Keeping the temperature of the fluorination kettle 6 at 95 ℃, putting the 2-chloro-3-trichloromethylpyridine into the fluorination kettle 6 through a fifth discharge hole 52 and a sixth feed hole 63, after the feeding is finished, increasing the temperature of the fluorination kettle 6 to 195 ℃, keeping the pressure at 5MPa, introducing 2827g of hydrogen fluoride from a hydrogen fluoride introduction hole 61, and reacting for 12 hours to obtain a reaction product; after the reaction is finished, cooling, slowly discharging pressure for 10 hours, expelling acid gas by using nitrogen, pressing materials by using nitrogen, and reducing the reaction pressure to normal pressure; and (3) putting the reaction product into a neutralization kettle 7 through a sixth discharge hole 62 and a seventh feed hole 73, adding water accounting for 105% of the mass of the reaction product into the reaction product through a water inlet 71, adding sodium hydroxide through an alkali inlet 74 to adjust the pH of the reaction system to 7, removing hydrogen fluoride and hydrogen chloride, and standing for layering to obtain a crude fluorinated product.
(3) Putting the fluorinated crude product into a second rectifying device 8 through a seventh discharge hole 72 and an eighth feed hole 81, and firstly, carrying out crystallization treatment on the fluorinated crude product to obtain a separated and purified product; and then, carrying out reduced pressure rectification on the separated and purified product, wherein the pressure of the reduced pressure rectification is kept at-0.99 Mpa, and the temperature of the circulating water of the condenser is 35 ℃. And collecting 100 ℃ fractions, finally collecting 814.0g of 2-chloro-3-trifluoromethylpyridine from a finished product discharge hole 82, and analyzing by gas chromatography, wherein the yield is 80.3% and the content is 99.1%.
The above description is only for the specific embodiments of the present invention, but the protection scope of the present invention is not limited thereto, and any person skilled in the art can easily think of the changes or substitutions within the technical scope of the present invention, and all should be covered within the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. A2-chloro-3-trifluoromethylpyridine synthesis device is characterized by comprising a multistage chlorination kettle, a first rectification device (4), a crystallization kettle (5), a fluorination kettle (6), a neutralization kettle (7) and a second rectification device (8) which are communicated in sequence;
the multistage chlorination kettle comprises more than two stages of chlorination kettles.
2. The apparatus for synthesizing 2-chloro-3-trifluoromethylpyridine according to claim 1, wherein the multistage chlorination reactor comprises a first-stage chlorination reactor (3), a second-stage chlorination reactor (2), and a third-stage chlorination reactor (1);
the upper end of the third-stage chlorination kettle (1) is provided with a first feeding hole (110), and the lower end of the third-stage chlorination kettle is provided with a first discharging hole (120);
the upper end of the secondary chlorination kettle (2) is provided with a second feeding hole (21) and a first material pouring hole (23), and the lower end is provided with a second discharging hole (22);
the upper end of the primary chlorination kettle (3) is provided with a third feeding port (31), a second material pouring port (33) and a chlorine introducing port (34), and the lower end is provided with a third discharging port (32);
a first chlorine channel (9) is arranged between the third-stage chlorination kettle (1) and the second-stage chlorination kettle (2), and a second chlorine channel (10) is arranged between the second-stage chlorination kettle (2) and the first-stage chlorination kettle (3);
first discharge gate (120) and first material pouring mouth (23) intercommunication setting, second discharge gate (22) and second material pouring mouth (33) intercommunication setting.
3. The apparatus for the synthesis of 2-chloro-3-trifluoromethylpyridine according to claim 2, characterized in that the first rectification device (4) is provided with a fourth inlet (41) and a fourth outlet (42); the fourth feed inlet (41) is communicated with the third discharge outlet (32).
4. The apparatus for synthesizing 2-chloro-3-trifluoromethylpyridine according to claim 3, wherein the crystallization kettle (5) is provided with a fifth inlet (51) and a fifth outlet (52); and the fifth feeding hole (51) is communicated with the fourth discharging hole (42).
5. The apparatus for synthesizing 2-chloro-3-trifluoromethylpyridine according to claim 4, wherein the fluorination reactor is provided with a hydrogen fluoride inlet (61), a sixth outlet (62), and a sixth inlet (63); and the sixth feeding hole (63) is communicated with the fifth discharging hole (52).
6. The apparatus for synthesizing 2-chloro-3-trifluoromethylpyridine according to claim 5, wherein the neutralization kettle (7) is provided with a water inlet (71), a seventh outlet (72), a seventh inlet (73), and a base inlet (74); and the seventh feeding hole (73) is communicated with the sixth discharging hole (62).
7. The apparatus for the synthesis of 2-chloro-3-trifluoromethylpyridine according to claim 6, characterized in that the second rectification device (8) is provided with an eighth inlet (81) and a finished product outlet (82); and the eighth feeding hole (81) is communicated with the seventh discharging hole (72).
8. The synthesis device of 2-chloro-3-trifluoromethylpyridine according to claim 2, wherein the three-stage chlorination kettle (1), the two-stage chlorination kettle (2), the one-stage chlorination kettle (3), the crystallization kettle (5), the fluorination kettle (6) and the neutralization kettle (7) are all provided with stirring devices (11).
9. The apparatus for synthesizing 2-chloro-3-trifluoromethylpyridine according to claim 2, wherein a reflux pipeline (12) is provided between the first chlorination reactor (3) and the first rectification apparatus (4).
10. The synthesis device of 2-chloro-3-trifluoromethylpyridine according to claim 2, wherein the three-stage chlorination kettle (1), the crystallization kettle (5) and the fluorination kettle (6) are provided with a tail gas absorption device; the second rectifying device (8) is provided with a reaction byproduct collecting device.
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