CN205603488U - A high -pressure consecutive reaction system for producing 3, 6 - dichloro salicylic acid - Google Patents
A high -pressure consecutive reaction system for producing 3, 6 - dichloro salicylic acid Download PDFInfo
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- CN205603488U CN205603488U CN201620385890.7U CN201620385890U CN205603488U CN 205603488 U CN205603488 U CN 205603488U CN 201620385890 U CN201620385890 U CN 201620385890U CN 205603488 U CN205603488 U CN 205603488U
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Abstract
The utility model relates to a production 3, 6 the high -pressure consecutive reaction system of dichloro salicylic acid belongs to the midbody technical field of synthetic weed killer mediben. This system is including the batching cauldron, carbon dioxide absorption cauldron, high -pressure conversion zone and the pressure release ejection of compact section that connect gradually, the high pressure conversion zone is including reaction pipeline and the blender of setting on the reaction pipeline, pressure release ejection of compact section is including the relief valve, buffer tank, condenser, acidizing cauldron and the filter pressing device that connect gradually. This system is serialization production 3, 6 expeditiously the dichloro salicylic acid.
Description
Technical field
This utility model relates to the production equipment of a kind of key intermediate for synthesizing Mediben, more specifically, this utility model relates to a kind of for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, belongs to the intermediate technical field of synthetic herbicide Mediben.
Background technology
Generally synthesis 3, the technique of 6-dichlorosalicylic acid uses still reaction, and reaction unit is autoclave, the most in the basic conditions, 2,5-chlorophenesic acids form phenates, and then solvent bank water is to aqueous below the 50ppm of system, proceed to autoclave again, add potassium carbonate catalyst, be passed through CO2Carry out carboxylation reaction, generate 3,6-dichlorosalicylic acid salt, then after reactant mixture being added water stratification, aqueous phase product adds acid and is acidified, vapor distillation separation and recovery unreacted 2,5-chlorophenesic acid, sucking filtration is dried and is then obtained pure 3,6-dichlorosalicylic acid solid.Being solvent high pressure carboxylation method, klobe-schitt reacts.In this technique, below carboxylation reaction material system water content 50ppm, technological requirement is high, and difficulty is big；The carboxylation reaction time is long, and coking is serious, and product yield is low, is only about 45%；High-temperature high-pressure apparatus and relevant auxiliary facility investment demand are high.It addition, prior art cannot realize 3, the continuous prodution of 6-dichlorosalicylic acid.
State Intellectual Property Office discloses Publication No. CN103012124A in 2013.4.3, the invention of entitled " 3; preparation method of the chloro-2 hydroxybenzoic acid of 6-bis-", this disclosure of the invention a kind of 3, the preparation method of the chloro-2 hydroxybenzoic acid of 6-bis-, comprise the following steps successively: 1) 2,5-chlorophenesic acid becomes salt；2) carboxylation: by 2,5-chlorophenesic acid saline solution is transferred in autoclave, adds co-catalyst, then passes to CO2 and carry out high pressure carboxylation reaction, must be containing 3, the product of 6-bis-chloro-2 hydroxybenzoic acid salt；Co-catalyst is made up of potassium carbonate and activated carbon；3) refined: by step 2) gained containing 3, after the product of 6-bis-chloro-2 hydroxybenzoic acid salt is cooled to room temperature, add aqueous slkali, regulate pH to 11 ~ 13, stir, activated carbon is recovered by filtration, phase of fetching water after filtrate layering；Adding acid solution in aqueous phase, regulate pH to 1 ~ 3, reclaim 2 through steam distillation, after 5-chlorophenesic acid, crystallisation by cooling, sucking filtration are dried, and obtain 3, the chloro-2 hydroxybenzoic acid of 6-bis-.Utilizing potassium carbonate and activated carbon co-catalyst in this method, reduce the consumption of potassium carbonate, reduce cost, but the response time is long, once through yield is low, and simply about 46%；
State Intellectual Property Office discloses Publication No. CN104086393A in 2014.10.8, the invention of entitled " the 3 of a kind of improvement; the preparation method of 6-dichlorosalicylic acid ", this disclosure of the invention 3 of a kind of improvement, the preparation method of 6-dichlorosalicylic acid, step is: by 2, and 5-chlorophenesic acid and alkaline reaction are subsequently adding organic solvent decompression dehydration；Add potassium carbonate, dehydrant and stabilizer after dehydration, react 30-60 minute at 130-140 DEG C；Material is added autoclave, is warming up to 130-140 DEG C, then pass to CO2 and carry out high pressure carboxylation reaction；Carry out post processing after reaction, obtain 3,6-dichlorosalicylic acid.The present invention is starvation before dehydration, carboxylation, avoid the oxygen oxidation to product, dehydrant and stabilizer is added before carboxylation, the hydrogen radical cation generated when eliminating the water in system and carboxylation further, maintain system stability, ensure that yield and be substantially improved product appearance, reducing the consumption of potassium carbonate, simplify last handling process.Additionally, the method is relatively low to the change of equipment, facilitating current manufacturing enterprise to implement to improve, can comparatively fast take effect benefit.In the method, the carboxylation reaction time is long, and reactant selectivity is low by about 94%, and complex process, and production cost is high.
State Intellectual Property Office discloses Publication No. CN102942474A in 2013.2.27, the invention of entitled " synthesis technique of a kind of herbicide dicamba ", this disclosure of the invention preparation method of a kind of herbicide dicamba, including: (1) liquid potassium hydroxide and 2,5-chlorophenesic acid obtains 2 with the molar ratio reaction of 0.95:1 ~ 1:1,5-chlorophenesic acid potassium；(2) the 2 of step (1) gained, 5-chlorophenesic acid potassium, in the presence of Anhydrous potassium carbonate and catalyst, reacts production 3,6-dichlorosalicylic acid with CO2；The pressure controlling CO2 is 4 ~ 6MPa, and reaction temperature 100 ~ 160 DEG C, Anhydrous potassium carbonate and 2, the mol ratio of 5-chlorophenesic acid potassium is 1 ~ 2:1；(3) in the basic conditions, at a temperature of 70 ~ 100 DEG C, by step (2) gained 3,6-dichlorosalicylic acid and chloromethanes press the mol ratio of 1:1 ~ 3.5 through calandria type fixed bed reactor, react under the effect of catalyst, 3 are obtained again through saponification, acidifying, 6-bis-chloro-2-methoxysalicylic acid, i.e. Mediben.The technological reaction yield of the present invention is high, reaction condition is simple, good product quality, the three wastes are few, energy consumption is low.
Above-mentioned three prior art literature disclose 3, the production technology of 6-dichlorosalicylic acid, but all cannot realize 3, the high efficiency of 6-dichlorosalicylic acid, continuous prodution.
Utility model content
This utility model aims to solve the problem that existing 3,6-dichlorosalicylic acid produce cannot realize serialization problem, it is provided that a kind of for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is possible to continuous prodution 3 expeditiously, 6-dichlorosalicylic acid.
In order to realize foregoing invention purpose, its concrete technical scheme is as follows:
It is a kind of for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: include batching kettle, carbon dioxide absorption still, reaction under high pressure section and the pressure release discharging section being sequentially connected with；Described reaction under high pressure section includes reacting pipe and the blender being arranged on reacting pipe, and described pressure release discharging section includes relief valve, surge tank, condenser, acidifying still and the filter-pressing device being sequentially connected with.
Batching kettle described in the utility model is connected with described carbon dioxide absorption still by dosing pump, described carbon dioxide absorption still is connected with described reaction under high pressure section by dosing pump, described reaction under high pressure section is connected with described surge tank further through described relief valve, described surge tank one end with described condenser again is connected, the other end of described condenser connects described acidifying still, and described acidifying still is connected with described filter-pressing device again.
Carbon dioxide absorption still described in the utility model forms a unit with described reaction under high pressure section, and this unit is two or more, is connected in series with each other.
Carbon dioxide absorption still described in the utility model is two or more, is connected in series with each other.
Reaction under high pressure section described in the utility model is two or more, is connected in series with each other.
Connected by dosing pump between above-mentioned reaction under high pressure section.
Absorption kettle heater, absorption kettle chiller, level display device, attemperating unit, pressure control device and pressure-display device it is provided with on carbon dioxide absorption still described in the utility model.
Blender described in the utility model is static mixer.
Blender described in the utility model is two or more.
It is provided with heater in reaction under high pressure section described in the utility model.
The Advantageous Effects that this utility model brings:
1, this utility model solves existing 3,6-dichlorosalicylic acid produce cannot realize serialization problem, it is provided that a kind of for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is possible to continuous prodution 3 expeditiously, 6-dichlorosalicylic acid.
2, this utility model uses continuous reacting device, greatly reduce reaction mass to turn material and get the raw materials ready the time, gas displacement process, remove reactant last handling process, reduce whole operation process, reduce a large amount of high-temperature high-pressure reaction kettle, reduce place capacity, it is easy to accomplish industrial automatic control, reduce artificial input, reduce equipment investment expense, reduce floor space, save space.
3, in continuous reaction apparatus of the present utility model, carbon dioxide absorption still can be effectively ensured in reaction required amount of carbon dioxide；Blender ensures solid-liquid-gas three phase reaction system mix homogeneously, improves reaction effect and intensified response efficiency, it is to avoid coking etc..
4, the setting of this utility model certain high pressure conversion zone, it is ensured that response time and the reduction reaction mass of reaction mass are detained or back-mixing in reaction unit.
5, this utility model is owing to, in course of reaction, pressure is change, and pump provides power for Flow of Goods and Materials, prevents material from high pressure to low pressure or refluence.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
Fig. 2 is this utility model carbon dioxide absorption still and reaction under high pressure segment unit is structural representation when two.
Fig. 3 is structural representation when this utility model two carbon dioxide absorption stills of existence and two reaction under high pressure section (one of them reaction under high pressure section arrange two blenders).
Reference: 1 be batching kettle, 2 be carbon dioxide absorption still, 3 be reacting pipe, 4 be blender, 5 be relief valve, 6 be surge tank, 7 be condenser, 8 be acidifying still, 9 be filter-pressing device, 10 for heater.
Detailed description of the invention
Embodiment 1
A kind of for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, including the batching kettle 1 being sequentially connected with, carbon dioxide absorption still 2, reaction under high pressure section and pressure release discharging section；Described reaction under high pressure section includes reacting pipe 3 and the blender 4 being arranged on reacting pipe 3, and described pressure release discharging section includes relief valve 5, surge tank 6, condenser 7, acidifying still 8 and the filter-pressing device 9 being sequentially connected with.
The course of reaction using above-mentioned high pressure continuous reaction system is:
A, in batching kettle 1 by 2, the xylene solution of 5-chlorophenesic acid potassium, Anhydrous potassium carbonate powder, dispersant stirring and evenly mixing, obtain slip；
B, the slip in step A is pumped into carbon dioxide absorption still 2 by dosing pump, open carbon dioxide air source, carry out carbon dioxide absorption, then slip pumps into reaction under high pressure section through dosing pump and reacts, and described reaction under high pressure section includes reacting pipe 3 and the blender 4 being arranged on reacting pipe 3；
C, the slip reacted through reaction under high pressure section, enter pressure release discharging section, described pressure release discharging section includes relief valve 5, surge tank 6, condenser 7, acidifying still 8 and the filter-pressing device 9 being sequentially connected with, and slip enters surge tank 6 after relief valve 5 pressure release, then cools down through condenser 7, acidifying still 8 is acidified, filter pressing, washing obtains 3,6-dichlorosalicylic acid wet product, finally it is dried to obtain 3,6-dichlorosalicylic acid product.
Embodiment 2
A kind of for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, including the batching kettle 1 being sequentially connected with, carbon dioxide absorption still 2, reaction under high pressure section and pressure release discharging section；Described reaction under high pressure section includes reacting pipe 3 and the blender 4 being arranged on reacting pipe 3, and described pressure release discharging section includes relief valve 5, surge tank 6, condenser 7, acidifying still 8 and the filter-pressing device 9 being sequentially connected with.
Described batching kettle 1 is connected with described carbon dioxide absorption still 2 by dosing pump, described carbon dioxide absorption still 2 is connected with described reaction under high pressure section by dosing pump, described reaction under high pressure section is connected with described surge tank 6 further through described relief valve 5, described surge tank 6 one end with described condenser 7 again is connected, the other end of described condenser 7 connects described acidifying still 8, and described acidifying still 8 is connected with described filter-pressing device 9 again.
Embodiment 3
On the basis of embodiment 1-2:
Preferably, described carbon dioxide absorption still 2 forms a unit with described reaction under high pressure section, and this unit is two or more, is connected in series with each other.
Preferably, described carbon dioxide absorption still 2 is two or more, is connected in series with each other.
Preferably, described reaction under high pressure section is two or more, is connected in series with each other.Further, connected by dosing pump between described reaction under high pressure section.
Preferably, described carbon dioxide absorption still 2 is provided with absorption kettle heater, absorption kettle chiller, level display device, attemperating unit, pressure control device and pressure-display device.
Preferably, described blender 4 is static mixer.
Preferably, described blender 4 is two or more.
Preferably, described reaction under high pressure section is provided with heater 10.
Claims (10)
1. one kind is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: include batching kettle (1), carbon dioxide absorption still (2), reaction under high pressure section and the pressure release discharging section being sequentially connected with；Described reaction under high pressure section includes reacting pipe (3) and the blender (4) being arranged on reacting pipe (3), and described pressure release discharging section includes relief valve (5), surge tank (6), condenser (7), acidifying still (8) and the filter-pressing device (9) being sequentially connected with.
One the most according to claim 1 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterized in that: described batching kettle (1) is connected with described carbon dioxide absorption still (2) by dosing pump, described carbon dioxide absorption still (2) is connected with described reaction under high pressure section by dosing pump, described reaction under high pressure section is connected with described surge tank (6) further through described relief valve (5), described surge tank (6) one end with described condenser (7) again is connected, the other end of described condenser (7) connects described acidifying still (8), described acidifying still (8) is connected with described filter-pressing device (9) again.
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterized in that: described carbon dioxide absorption still (2) forms a unit with described reaction under high pressure section, and this unit is two or more, is connected in series with each other.
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: described carbon dioxide absorption still (2) is two or more, is connected in series with each other.
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: described reaction under high pressure section is two or more, is connected in series with each other.
One the most according to claim 5 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: connected by dosing pump between described reaction under high pressure section.
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: it is provided with absorption kettle heater, absorption kettle chiller, level display device, attemperating unit, pressure control device and pressure-display device on described carbon dioxide absorption still (2).
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: described blender (4) is static mixer.
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: described blender (4) is two or more.
One the most according to claim 1 and 2 is used for production 3, the high-pressure continuous reaction system of 6-dichlorosalicylic acid, it is characterised in that: it is provided with heater (10) in described reaction under high pressure section.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620385890.7U CN205603488U (en) | 2016-05-03 | 2016-05-03 | A high -pressure consecutive reaction system for producing 3, 6 - dichloro salicylic acid |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201620385890.7U CN205603488U (en) | 2016-05-03 | 2016-05-03 | A high -pressure consecutive reaction system for producing 3, 6 - dichloro salicylic acid |
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