CN208898769U - Acyl chlorides product production system - Google Patents

Acyl chlorides product production system Download PDF

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CN208898769U
CN208898769U CN201821615481.7U CN201821615481U CN208898769U CN 208898769 U CN208898769 U CN 208898769U CN 201821615481 U CN201821615481 U CN 201821615481U CN 208898769 U CN208898769 U CN 208898769U
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pipeline
tank
chloride
film
tower
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黎孔富
孙大明
黎长健
方明祥
方容
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YIDU YOUYUAN INDUSTRIAL Co Ltd
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YIDU YOUYUAN INDUSTRIAL Co Ltd
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Abstract

The utility model relates to acyl chlorides product production systems, including crude synthesis reactor, it is connected to by pipeline with dropping tank above the crude synthesis reactor, the first destilling tower is equipped at the top of the crude synthesis reactor, it is sequentially connected at the top of first destilling tower by pipeline and the first condenser, gas-liquid separator, collecting tank, the gas-liquid separator bottom is by pipeline by being connected at the top of return valve and the first destilling tower.Using isobutyric acid and benzotrichloride as raw material, isobutyryl chloride and chlorobenzoyl chloride product are produced using coproduction scheme, carry out distillation separation, in crude heating synthesis process, reaction is continuously generated low boiling material (isobutyryl chloride), it is increased with synthesis temperature, low boiling material (isobutyryl chloride) is largely evaporated, and is gradually separated and collected product (isobutyryl chloride), using same set of equipment, be conducive to material sufficiently to react, finished product can be distilled rapidly to obtain by generating isobutyryl chloride.The utility model has the advantages that process route is simple, easy to operate, " three wastes " discharge amount is few.

Description

Acyl chlorides product production system
Technical field
The utility model relates to organic compound preparation method field, especially a kind of acyl chlorides product production system.
Background technique
Isobutyryl chloride is also known as: chlorination isobutyryl, 2- methyl propionyl chloride,
Its purposes is very extensive, is used as organic synthesis intermediate, is the raw material for producing efficient photoinitiator PI-906, PI-907. Conventional isobutyryl chloride preparation process is to use isobutyric acid in the presence of a catalyst, is carried out with thionyl chloride or phosphorus oxychloride acylated anti- It answers, after the reaction was completed, using distillating method by isobutyryl chloride distilation, obtains product, react residual chloride sulfoxide or trichlorine oxygen Phosphorus and waste liquid are handled with water decomposition, and wastewater flow rate is big, and environmental pollution is serious, and reaction process is complicated for operation.
Summary of the invention
In order to overcome aforesaid operations complicated, problem that environmental pollution is serious.The utility model provides a kind of acyl chlorides production System carries out isobutyryl chloride production using co-production, and in the synthesis process, isobutyryl chloride is constantly steamed, qualification is obtained Product, one step of the method can obtain qualified isobutyryl chloride, do not need synthesis after again rectifying collect isobutyryl chloride, it is easy to operate, Loss of material is small, non-environmental-pollution.
In order to solve the above technical problems, the technical scheme adopted by the utility model is:
A kind of acyl chlorides product production system, including crude synthesis reactor, the crude synthesis reactor top is by pipeline and is added dropwise Tank connection, the crude synthesis reactor top are equipped with the first destilling tower, pass through pipeline and the first condensation at the top of first destilling tower Device, gas-liquid separator, collecting tank are sequentially connected, and return valve and the first destilling tower are passed through by pipeline in the gas-liquid separator bottom Top connection.
Preferably, the collecting tank is isobutyryl chloride collecting tank.
Preferably, the gas-liquid separator is connected to by pipeline with film-falling absorption tower, the falling film absorption tower bottom and salt Sour tourie connection, the top film-falling absorption tower are connected to by circulating pump with absorption by Hydrochloric Acid tank, and the film-falling absorption tower passes through Pipeline is connected to oil-sealed rotary pump.
It is further preferred that two film-falling absorption towers are connected in series there are two the film-falling absorption tower sets.
It is further preferred that the collecting tank is enamel storage tank, the absorption by Hydrochloric Acid tank volume is 25m3;The falling liquid film Absorption tower is graphite film-falling absorption tower, volume 20m2, the circulation pump power is 3KW.
Preferably, the crude synthesis reactor is connected to benzoyl chloride distillation pot by pipeline by pipeline, the benzoyl After-fractionating tower is equipped at the top of chlorine distillation still, the after-fractionating top of tower is connected to by pipeline with the second condenser, and described the Two condensers pass through respectively pipeline with before evaporate tank, chlorobenzoyl chloride finished pot is connected to, tank is evaporated before described and passes through pipeline and crude synthesis Kettle connection.
Using the technique of the system production isobutyryl chloride, response path is as follows:
The technique the following steps are included:
1) benzotrichloride is put into crude synthesis reactor, catalyst is added, is warming up to 90-120 DEG C, dropping tank starts to drip After adding isobutyric acid, reaction to start, material uses infinite reflux in the first destilling tower when having material to start to be evaporated in the first destilling tower Operation, after reacting 30 minutes, material regurgitant volume increases, and reduces reflux ratio, and sample detection isobutyryl chloride content (isobutyryl chloride 90.9 DEG C of boiling point), start to collect isobutyryl chloride after reaching quality standards, benzotrichloride is ensured using continuous backflow during collecting Finished product is not brought into chlorobenzoyl chloride;
2) hydrogen chloride gas of reaction production is absorbed using two-stage film-falling absorption tower, and absorption prepares hydrochloric acid;
3) the crude material in reactor of sample detection, which reaches, after having reacted goes to chlorobenzoyl chloride distillation after crude product quality requires Kettle (10) distillation;
4), benzoyl chloride distillation pot distills initial stage, and by material collection to before evaporating in tank, ingredient is isobutyryl chloride and benzene first Acyl chlorides mixed material is collected after distillation to chlorobenzoyl chloride qualification to chlorobenzoyl chloride finished pot;
5) mixed material collected in tank is evaporated before and is brought into crude synthesis reactor in next batch is distilled separation again Processing;
The technique for completing isobutyryl chloride.
It is further preferred that the step 1) catalyst is lewis acid, the step 1) is warming up to 90-120 DEG C, institute Stating step 1) quality standard is that isobutyryl chloride content is greater than 99.00%.
It is further preferred that the step 3) crude product quality requires to be material in reactor benzotrichloride≤0.3%, isobutyl Acid≤0.5%;Step 4) the benzoyl chloride distillation pot distillation initial stage is chlorobenzoyl chloride content less than 99.00%.
The system can also be used in the production that the boiling points such as chloracetyl chloride, chloroacetic chloride or acryloyl chloride are less than crude synthesis temperature Product production.
The utility model has following technical effect that
1, the utility model is suitable for acyl chlorides system product production of the boiling temperature within 120 DEG C.With isobutyric acid and three Chlorotoluene is raw material, produces isobutyryl chloride and chlorobenzoyl chloride product using coproduction scheme, carries out distillation separation, crude heating synthesis In the process, reaction is continuously generated low boiling material (isobutyryl chloride), increases with synthesis temperature, and low boiling material (isobutyryl chloride) is big Amount evaporation, gradually separates and collects product (isobutyryl chloride), using same set of equipment, this reaction is closed at 100-120 DEG C At synthesis temperature is more than isobutyryl chloride material evaporation temperature, and material is constantly evaporated discharge during the reaction, is conducive to object Material sufficiently reaction, finished product can be distilled rapidly to obtain by generating isobutyryl chloride.The utility model have process route it is simple, it is easy to operate, Prepare the advantage that facility is few, " three wastes " discharge amount is few.
2, corresponding acyl chlorides and chlorobenzoyl chloride under the action of catalyst with benzotrichloride and organic acid, can be synthesized, in order to Two different acyl chlorides products are more preferably separated, are separated using distillation, distillation separation selection boiling temperature differs larger, ability It efficiently separates.
3, the utility model carries out isobutyryl chloride production using co-production, and in the synthesis process, not by isobutyryl chloride It is disconnected to steam, qualified products are obtained, one step of the method can obtain qualified isobutyryl chloride, not need after synthesis that isobutyl is collected in rectifying again Acyl chlorides, easy to operate, loss of material is small, non-environmental-pollution.
4, a dropping tank is installed on crude synthesis reactor, controls reaction speed, in the case where controlling temperature conditions, is uniformly dripped Add, guarantees stable reaction.
5, on crude synthesis reactor, condenser is repacked into first destilling tower, top of tower installs the first condenser, carries out object Reflux is collected in material condensation, and the isobutyryl chloride for reacting generation directly distills collection.
6, gas-liquid separator is installed in condenser, gas phase is discharged into followed by absorption.The installation of gas-liquid separator lower part Return valve flows back.Return valve is installed on the first destilling tower, according to control of product quality reflux size, guarantees product It is up-to-standard.
7, according to crude synthesis input quantity, an isobutyryl chloride collecting tank is installed, carries out the collection of isobutyryl chloride product.
8, hydrochloric acid is made using film-falling absorption tower absorption in tail gas hydrogen chloride gas, using oil-sealed rotary pump to whole system shape At micro-vacuum.
Detailed description of the invention
The utility model is described in further detail with reference to the accompanying drawings and examples:
Fig. 1 is the structural schematic diagram of the utility model.
In figure: crude synthesis reactor 1, dropping tank 2, the first destilling tower 3, the first condenser 4, gas-liquid separator 5, collecting tank 6, Return valve 7, benzoyl chloride distillation pot 8, after-fractionating tower 9, the second condenser 10 are preceding to evaporate tank 11, chlorobenzoyl chloride finished pot 12, drop Film absorption tower 13, oil-sealed rotary pump 14, circulating pump 16.
Specific embodiment
Embodiment 1
A kind of acyl chlorides product production system, including crude synthesis reactor 1 pass through pipeline and drop above the crude synthesis reactor 1 Add tank 2 to be connected to, be equipped with the first destilling tower 3 at the top of the crude synthesis reactor 1, passes through pipeline and the at the top of first destilling tower 3 One condenser 4, gas-liquid separator 5, collecting tank 6 are sequentially connected, and return valve 7 is passed through by pipeline in 5 bottom of gas-liquid separator It is connected to at the top of the first destilling tower 3.
Preferably, the collecting tank 6 is isobutyryl chloride collecting tank.
Preferably, the gas-liquid separator 5 is connected to by pipeline with film-falling absorption tower 13,13 bottom of film-falling absorption tower Portion is connected to absorption by Hydrochloric Acid tank 15, and the top film-falling absorption tower 13 is connected to by circulating pump 16 with absorption by Hydrochloric Acid tank 15, described Film-falling absorption tower 13 is connected to by pipeline with oil-sealed rotary pump 14.
It is further preferred that two film-falling absorption towers 13 are connected in series there are two the film-falling absorption tower 13 sets.
It is further preferred that the collecting tank 6 is enamel storage tank, 15 volume of absorption by Hydrochloric Acid tank is 25m3;It is described Film-falling absorption tower 13 is graphite film-falling absorption tower, volume 20m2, 16 power of circulating pump is 3KW.
Preferably, the crude synthesis reactor 1 is connected to benzoyl chloride distillation pot 8 by pipeline by pipeline, the benzene first It is equipped with after-fractionating tower 9 at the top of acyl chlorides distillation still 8, is connected to by pipeline with the second condenser 10 at the top of the after-fractionating tower 9, Second condenser 10 respectively by pipeline with before evaporate tank 11, chlorobenzoyl chloride finished pot 12 is connected to, tank 11 is evaporated before described and is passed through Pipeline is connected to crude synthesis reactor 1.
Embodiment 2
A kind of acyl chlorides product production system, including crude synthesis reactor 1 pass through pipeline and drop above the crude synthesis reactor 1 Add tank 2 to be connected to, be equipped with the first destilling tower 3 at the top of the crude synthesis reactor 1, passes through pipeline and the at the top of first destilling tower 3 One condenser 4, gas-liquid separator 5, collecting tank 6 are sequentially connected, and return valve 7 is passed through by pipeline in 5 bottom of gas-liquid separator It is connected to at the top of the first destilling tower 3.
Preferably, the collecting tank 6 is isobutyryl chloride collecting tank.
Preferably, the gas-liquid separator 5 is connected to by pipeline with film-falling absorption tower 13,13 bottom of film-falling absorption tower Portion is connected to absorption by Hydrochloric Acid tank 15, and the top film-falling absorption tower 13 is connected to by circulating pump 16 with absorption by Hydrochloric Acid tank 15, described Film-falling absorption tower 13 is connected to by pipeline with oil-sealed rotary pump 14.
It is further preferred that two film-falling absorption towers 13 are connected in series there are two the film-falling absorption tower 13 sets.
It is further preferred that the collecting tank 6 is enamel storage tank, 15 volume of absorption by Hydrochloric Acid tank is 25m3;It is described Film-falling absorption tower 13 is graphite film-falling absorption tower, volume 20m2, 16 power of circulating pump is 3KW.
Preferably, the crude synthesis reactor 1 is connected to benzoyl chloride distillation pot 8 by pipeline by pipeline, the benzene first It is equipped with after-fractionating tower 9 at the top of acyl chlorides distillation still 8, is connected to by pipeline with the second condenser 10 at the top of the after-fractionating tower 9, Second condenser 10 respectively by pipeline with before evaporate tank 11, chlorobenzoyl chloride finished pot 12 is connected to, tank 11 is evaporated before described and is passed through Pipeline is connected to crude synthesis reactor 1.
Using the technique of the system production isobutyryl chloride, response path is as follows:
The technique the following steps are included:
1) benzotrichloride is put into crude synthesis reactor 1, catalyst is added, is warming up to 90-120 DEG C, dropping tank 2 is opened Begin that isobutyric acid is added dropwise, after reaction starts, material is used in first destilling tower 3 when having material to start to be evaporated in the first destilling tower 3 Total reflux operation, after reacting 30 minutes, material regurgitant volume increases, and reduces reflux ratio, and sample detection isobutyryl chloride content is (different 90.9 DEG C of butyl chloride boiling point), start to collect isobutyryl chloride after reaching quality standards, ensures three using continuous backflow during collecting Chlorotoluene and chlorobenzoyl chloride do not bring finished product into;
2) hydrogen chloride gas of reaction production is absorbed using two-stage film-falling absorption tower 13, and absorption prepares hydrochloric acid;
3) the crude material in reactor of sample detection, which reaches, after having reacted goes to chlorobenzoyl chloride distillation after crude product quality requires Kettle 10 distills;
4), benzoyl chloride distillation pot distills initial stage, and by material collection to before evaporating 11 in tank, ingredient is isobutyryl chloride and benzene Formyl chloride mixed material is collected after distillation to chlorobenzoyl chloride qualification to chlorobenzoyl chloride finished pot 12;
5) mixed materials that 11 collect are evaporated in tank before and are brought into crude synthesis reactor 1 in next batch is distilled again point From processing;
The technique for completing isobutyryl chloride.
It is further preferred that the step 1) catalyst is lewis acid, the step 1) is warming up to 90-120 DEG C, institute Stating step 1) quality standard is that isobutyryl chloride content is greater than 99.00%.
It is further preferred that the step 3) crude product quality requires to be material in reactor benzotrichloride≤0.3%, isobutyl Acid≤0.5%;Step 4) the benzoyl chloride distillation pot distillation initial stage is chlorobenzoyl chloride content less than 99.00%.
It is further preferred that the collecting tank 6 is enamel storage tank, 15 volume of absorption by Hydrochloric Acid tank is 25m3;It is described Film-falling absorption tower 13 is graphite film-falling absorption tower, volume 20m2, 16 power of circulating pump is 3KW.
The crude synthesis reactor 1 is connected to benzoyl chloride distillation pot 8 by pipeline by pipeline, the chlorobenzoyl chloride distillation It is equipped with after-fractionating tower 9 at the top of kettle 8, is connected to by pipeline with the second condenser 10 at the top of the after-fractionating tower 9, described second Condenser 10 respectively by pipeline with before evaporate tank 11, chlorobenzoyl chloride finished pot 12 be connected to, evaporated before described tank 11 by pipeline with slightly Synthesis reactor 1 processed is connected to.The crude synthesis reactor 1 uses 2000L enamel reaction still, and dropping tank 2 uses 1000L polypropylene plastics Tank, the first destilling tower 3 use enamel tower, and the first condenser 4 uses 20m2Graphite condenser, reflux control use glass valves Door control reflux size, collecting tank 6 use 2000L enamel storage tank, and absorption by Hydrochloric Acid uses a fiberglass-reinforced glass storage tank 25m3, two Graphite film-falling absorption tower 20m2An and 3KW HCl solution circulating pump.Gas-liquid separator is installed in condenser, after gas phase is discharged into Face is absorbed.5 lower part of gas-liquid separator installation return valve 7 flows back.Benzotrichloride is put into crude synthesis reactor 1 Catalyst is added in 1850kg, is warming up to 100 DEG C, and isobutyric acid is added dropwise, and rate of addition is determined according to reaction condition, until drop It adds into.Dropwise reaction initial stage, material use infinite reflux, and sample detection isobutyryl chloride content, start after reaching quality standards Isobutyryl chloride is collected, ensures that benzotrichloride does not bring finished product into using continuous backflow during collecting.React the hydrogen chloride gas of production Body is absorbed using two-stage serous coat absorption tower, and absorption prepares hydrochloric acid.Insulation reaction after dropwise reaction is complete, isobutyryl chlorine dose in kettle Infinite reflux is used when less, guarantees that the product collected is qualified.The crude material in reactor content of sample detection, reaches after having reacted Crude product quality goes to benzoyl chloride distillation pot distillation after requiring.Benzoyl chloride distillation pot distills initial stage, by material collection to before evaporating In tank, ingredient is isobutyryl chloride and chlorobenzoyl chloride mixed material, distillation to chlorobenzoyl chloride it is qualified after collect to chlorobenzoyl chloride at Product tank.Mixed material is brought into crude synthesis reactor in next batch and is handled.
Embodiment 3
Chloracetyl chloride production is carried out using system described in embodiment 1:
1) monoxone is put into crude synthesis reactor 1, catalyst is added, be warming up to 90-120 DEG C, dropping tank 2 starts Benzotrichloride is added dropwise, after reaction starts, has the generation of chloracetyl chloride material, as reaction temperature increases, has material to start to be evaporated to Material uses total reflux operation in first destilling tower 3 when in the first destilling tower 3, and after reaction temperature is more than 105 DEG C, material is returned Flow increases, and reduces reflux ratio, and sample detection chloracetyl chloride content (105 DEG C of chloracetyl chloride boiling point), reaches quality standards Start to collect chloracetyl chloride after (chloracetyl chloride content is greater than 99.00%), three chloromethanes are ensured using continuous backflow during collecting Benzene and chlorobenzoyl chloride do not bring finished product into;
2) hydrogen chloride gas of reaction production is absorbed using two-stage film-falling absorption tower 13, and absorption prepares hydrochloric acid;
3) the crude material in reactor of sample detection reaches crude product quality and requires that (benzotrichloride content is less than after having reacted 0.30%, monoxone is distilled less than benzoyl chloride distillation pot 10 is gone to after 0.50%);
4), benzoyl chloride distillation pot distills initial stage, and by material collection to before evaporating 11 in tank, ingredient is chloracetyl chloride and benzene Formyl chloride mixed material, distillation to chlorobenzoyl chloride qualified (chlorobenzoyl chloride content is greater than 99.00%) collect afterwards to chlorobenzoyl chloride at Product tank 12;
5) mixed materials that 11 collect are evaporated in tank before and are brought into crude synthesis reactor 1 in next batch is distilled again point From processing;
The technique for completing chloracetyl chloride.

Claims (6)

1. a kind of acyl chlorides product production system, including crude synthesis reactor (1), it is characterised in that: above the crude synthesis reactor (1) It is connected to by pipeline with dropping tank (2), is equipped with the first destilling tower (3) at the top of the crude synthesis reactor (1), first destilling tower (3) top is sequentially connected by pipeline with the first condenser (4), gas-liquid separator (5), collecting tank (6), the gas-liquid separator (5) bottom is by pipeline by being connected at the top of return valve (7) and the first destilling tower (3).
2. acyl chlorides product production system according to claim 1, it is characterised in that: the collecting tank (6) is isobutyryl chloride Collecting tank.
3. acyl chlorides product production system according to claim 1, it is characterised in that: the gas-liquid separator (5) passes through pipe Road is connected to film-falling absorption tower (13), and film-falling absorption tower (13) bottom is connected to absorption by Hydrochloric Acid tank (15), the top drop Film absorption tower (13) is connected to by circulating pump (16) with absorption by Hydrochloric Acid tank (15), and the film-falling absorption tower (13) passes through pipeline and machine Tool vacuum pump (14) connection.
4. acyl chlorides product production system according to claim 3, it is characterised in that: the film-falling absorption tower (13) is equipped with two A, two film-falling absorption towers (13) are connected in series.
5. acyl chlorides product production system according to claim 3, it is characterised in that: the collecting tank (6) is enamel storage Tank, the film-falling absorption tower (13) are graphite film-falling absorption tower.
6. acyl chlorides product production system according to claim 1, it is characterised in that: the crude synthesis reactor (1) passes through pipe Road is connected to benzoyl chloride distillation pot (8) by pipeline, is equipped with after-fractionating tower (9) at the top of the benzoyl chloride distillation pot (8), It is connected to by pipeline with the second condenser (10) at the top of the after-fractionating tower (9), second condenser (10) passes through respectively Pipeline with before evaporate tank (11), chlorobenzoyl chloride finished pot (12) is connected to, tank (11) are evaporated before described and pass through pipeline and crude synthesis reactor (1) Connection.
CN201821615481.7U 2018-09-30 2018-09-30 Acyl chlorides product production system Active CN208898769U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109081778A (en) * 2018-09-30 2018-12-25 宜都市友源实业有限公司 A kind of acyl chlorides product production system and technique

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109081778A (en) * 2018-09-30 2018-12-25 宜都市友源实业有限公司 A kind of acyl chlorides product production system and technique
CN109081778B (en) * 2018-09-30 2023-10-27 宜都市友源实业有限公司 System and process for producing acyl chloride product

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Denomination of utility model: Acyl chloride product production system

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Denomination of utility model: Acyl chloride product production system

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