CN211170524U - Preparation system of adipic acid dibasic ester - Google Patents

Preparation system of adipic acid dibasic ester Download PDF

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Publication number
CN211170524U
CN211170524U CN201922387872.9U CN201922387872U CN211170524U CN 211170524 U CN211170524 U CN 211170524U CN 201922387872 U CN201922387872 U CN 201922387872U CN 211170524 U CN211170524 U CN 211170524U
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stage
inlet
equipment
water separator
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刘涌
蔡健
张虎
郑玉婷
袁坚
戴祖红
吴逊
聂常洪
杨红
刘晓雯
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JIANGSU YIDA CHEMICAL CO Ltd
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JIANGSU YIDA CHEMICAL CO Ltd
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Abstract

The utility model relates to a preparation system of adipic acid dibasic ester, which comprises an esterification reaction stage, an esterification wastewater treatment stage, a dealcoholization stage, a distillation stage, a washing stage, a dehydration stage and a filtering stage; wherein, the equipment in the esterification reaction stage is as follows: a reaction kettle, a condenser and a water separator; the equipment in the esterification wastewater treatment stage comprises: a distillation kettle; the equipment in the dealcoholization stage is as follows: a dealcoholization tower; the distillation stage equipment was: a thin film evaporator; the equipment in the water washing stage is as follows: a water washing tank; the equipment in the dehydration stage is as follows: a dehydrator; the equipment in the filtration stage is: a filtering device and a finished product tank. The utility model discloses a preparation system adopts film evaporator to separate the refining, can get rid of the catalyst in the product effectively, improves product quality, and the setting of washing jar can get rid of some micro impurity that influence product quality fast effectively, and the product purity who obtains is high, can store for a long time, can neglect equipment corrosion, and also minimum to the pollution of environment.

Description

Preparation system of adipic acid dibasic ester
Technical Field
The utility model relates to a production facility technical field of ester compound, in particular to preparation system of adipic acid dibasic ester.
Background
The adipic acid dibasic ester compound is an important organic chemical product with wide application, and is commonly used in the fields of plasticizers, film-forming aids and other coatings. The traditional synthesis method of diisopropyl adipate is that adipic acid and isopropanol are subjected to direct catalytic reaction under the condition of a water-carrying agent, but a large amount of water-carrying agents existing in a system are difficult to remove, so that the energy consumption of a subsequent product separation process is increased.
Chinese patent publication No. CN102911048A utility model discloses a preparation method of diisobutyl adipate, provides and uses concentrated sulfuric acid as catalyst, through the washing, dealcoholize, refine, the preparation method of purification product such as filtration, but comes washing product through adding the refining agent and can introduce other impurity, influences the follow-up use of product, and traditional vacuum distillation of vacuum distillation and rectification equipment volume is bigger again to efficiency is not high.
In order to solve the above problems, the present applicant has previously developed a process for preparing adipic acid dibasic ester by research, and in order to complement the preparation process, the present applicant herein provides a system for preparing adipic acid dibasic ester.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a preparation system of adipic acid dibasic ester, in order to support the preparation technology of adipic acid dibasic ester that the applicant improved and filed the application.
In order to achieve the above purpose, the utility model provides a technical scheme as follows:
a preparation system of adipic acid dibasic ester comprises an esterification reaction stage, an esterification wastewater treatment stage, a dealcoholization stage, a distillation stage, a water washing stage, a dehydration stage and a filtering stage; wherein, the equipment in the esterification reaction stage is as follows: a reaction kettle, a condenser and a water separator; the equipment in the esterification wastewater treatment stage comprises: a distillation kettle; the equipment of the dealcoholization stage is as follows: a dealcoholization tower; the distillation stage equipment is: a thin film evaporator; the equipment in the water washing stage is as follows: a water washing tank; the equipment in the dehydration stage is as follows: a dehydrator; the equipment in the filtering stage is as follows: a filtering device and a finished product tank.
Furthermore, the side wall of the reaction section of the reaction kettle is provided with a raw material inlet, the top of the reaction kettle is provided with a gas phase outlet, the gas phase outlet is provided with a three-way valve, and the bottom of the reaction kettle is provided with a reaction liquid outlet;
the condenser comprises a condensation inlet and a condensation outlet, and the condensation inlet is connected with the gas phase outlet through a three-way valve;
the water separator comprises a water separator inlet, a water separator first outlet and a water separator second outlet, wherein the water separator inlet is connected with the condensation outlet through a pipeline, and the water separator first outlet is connected with the gas phase outlet through a three-way valve.
Further, the distillation still comprises a distillation still inlet connected with the second outlet of the water separator through a pipeline, an organic matter outlet at the top of the distillation still and a first wastewater outlet at the bottom of the distillation still.
Further, the dealcoholization tower comprises a reaction liquid inlet, a waste alcohol outlet and a crude product outlet, wherein the reaction liquid inlet is connected with the reaction liquid outlet through a pipeline.
Further, the film evaporator comprises a crude product inlet, a light component outlet and a heavy component outlet, wherein the crude product inlet is connected with the crude product outlet through a pipeline.
Further, the washing tank comprises a light component inlet, a water inlet and an upper product outlet, wherein the light component inlet is connected with the light component outlet through a pipeline.
Further, the dehydrator comprises an upper product inlet, a second wastewater outlet and a material outlet, wherein the upper product inlet is connected with the upper product outlet through a pipeline.
Furthermore, the inlet of the filtering device is connected with the material outlet, and the outlet of the filtering device is connected with the finished product tank through a pipeline.
Compared with the prior art, the utility model, its advantage lies in with beneficial effect:
the utility model discloses a preparation system adopts film evaporator to separate the refining, can get rid of the catalyst in the product effectively, improves product quality, gets rid of some micro impurity that influence product quality fast effectively through setting up of washing jar simultaneously, and the product purity who obtains is high, can store for a long time, can neglect equipment corrosion, and also minimum to the pollution of environment.
Drawings
FIG. 1 is a flow diagram of a process for the preparation of dibasic esters of adipic acid;
FIG. 2 is a schematic view of a preparation system according to an embodiment of the present invention;
reference numerals: the system comprises a reaction kettle 1, a condenser 2, a water separator 3, a distillation kettle 4, a dealcoholization tower 5, a thin film evaporator 6, a water washing tank 7, a dehydrator 8, a filtering device 9 and a finished product tank 10.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and specific embodiments.
In order to improve the difficulty and quality of product purification caused by adding a refining agent to wash a product and introducing other impurities in the existing preparation process of adipic acid dibasic ester, the applicant provides a preparation process of adipic acid dibasic ester through research and improvement, the process flow is shown in figure 1, a homogeneous catalyst is adopted, the reaction efficiency is improved due to high catalytic activity, then separation and refining are carried out by combining a thin-film evaporator, the catalyst in the product is effectively removed, the product quality is improved, meanwhile, impurities influencing the product quality are quickly and effectively removed through warm water washing, the obtained product is high in purity, can be stored for a long time, the corrosion to equipment is negligible, and the pollution to the environment is extremely small.
Meanwhile, in order to match with the preparation process of the adipic acid dibasic ester, the utility model provides a preparation system of adipic acid dibasic ester, which comprises an esterification reaction stage, an esterification wastewater treatment stage, a dealcoholization stage, a distillation stage, a water washing stage, a dehydration stage and a filtering stage, as shown in figure 1.
Wherein, the esterification reaction stage adopts the following equipment: a reaction kettle 1, wherein a raw material inlet is arranged on the side wall of the reaction section of the reaction kettle, a gas phase outlet is arranged on the top of the reaction kettle, a three-way valve (not shown in the figure) is arranged on the gas phase outlet, and a reaction liquid outlet is arranged at the bottom of the reaction kettle 1;
the condenser 2 comprises a condensation inlet and a condensation outlet, and the condensation inlet is connected with the gas phase outlet through a three-way valve;
and the water separator 3 comprises a water separator inlet, a first water separator outlet and a second water separator outlet, the water separator inlet is connected with the condensation outlet through a pipeline, and the first water separator outlet is connected with the gas phase outlet through a three-way valve.
The esterification wastewater treatment stage adopts the following equipment: and the distillation kettle 4 comprises a distillation kettle inlet connected with the second outlet of the water separator through a pipeline, an organic matter outlet at the top of the distillation kettle and a first wastewater outlet at the bottom of the distillation kettle.
The dealcoholization stage adopts the following equipment: and the dealcoholization tower 5 comprises a reaction liquid inlet, a waste alcohol outlet and a crude product outlet, wherein the reaction liquid inlet is connected with the reaction liquid outlet through a pipeline.
The distillation stage employs equipment that: and the thin film evaporator 6 comprises a crude product inlet, a light component outlet and a heavy component outlet, wherein the crude product inlet is connected with the crude product outlet through a pipeline.
The equipment adopted in the water washing stage is as follows: and the water washing tank 7 comprises a light component inlet, a water inlet and an upper product outlet, and the light component inlet is connected with the light component outlet through a pipeline.
The dehydration stage adopts the following equipment: the dehydrator 8 comprises an upper product inlet, a second wastewater outlet and a material outlet, wherein the upper product inlet is connected with the upper product outlet through a pipeline.
The filtration stage employs equipment that: the inlet of the filtering device 9 is connected with the material outlet, and the outlet is connected with a finished product tank 10 through a pipeline.
The utility model discloses a theory of operation: in the esterification reaction stage, raw materials required by the reaction are put into a reaction kettle 1 through a raw material inlet, stirred and heated to boiling reaction, reaction liquid steam enters a condenser 2 through a gas phase outlet through a condensation inlet, a part of the reaction liquid steam is precooled and liquefied and then returns to the reaction kettle along the original path, the other part of the reaction liquid steam enters a water separator 3 from a condensation outlet, the reaction liquid is separated into a water layer and an organic layer in the water separator 3, the organic layer liquid is returned to the reaction kettle for continuous reaction, the separated water and a small amount of organic matters enter the esterification wastewater treatment stage for treatment, when the reaction is not carried out, the heating is stopped, and the esterification reaction is finished; in the esterification wastewater treatment stage, water and a small amount of organic matters separated by the water separator 3 enter a distillation kettle 4 through a distillation kettle inlet to carry out distillation operation, and the organic matters are collected from an organic matter outlet at the top of the distillation kettle for recycling; collecting wastewater from a first wastewater outlet at the bottom of the distillation kettle for further treatment; in the dealcoholization stage, conveying the reaction liquid in the esterification reaction stage from a reaction liquid outlet at the bottom of the reaction kettle 1 to a dealcoholization tower 5 for dealcoholization operation to obtain a crude product and waste alcohol liquid, and collecting the waste alcohol liquid through a waste alcohol outlet to be treated in the next step; the crude product is sent into a thin film evaporator 6 for distillation, an intermediate product is obtained from a light component outlet of the thin film evaporator 6 and is collected into a rinsing tank 7, and a heavy component is collected from a heavy component outlet of the thin film evaporator for recycling; adding warm water into the water washing tank 7 to wash the intermediate product, standing for layering, collecting the upper product, putting into a dehydrator 8, decompressing and dehydrating, then sending the product into a filtering device 9 for filtering to obtain the final product, and collecting the final product to a finished product tank 10.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It should be understood that the present invention is not limited by the above embodiments, and the description in the above embodiments and the description is only for the purpose of illustrating the principles of the present invention, without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. A preparation system of adipic acid dibasic ester is characterized by comprising an esterification reaction stage, an esterification wastewater treatment stage, a dealcoholization stage, a distillation stage, a water washing stage, a dehydration stage and a filtering stage; wherein, the equipment in the esterification reaction stage is as follows: a reaction kettle, a condenser and a water separator; the equipment in the esterification wastewater treatment stage comprises: a distillation kettle; the equipment of the dealcoholization stage is as follows: a dealcoholization tower; the distillation stage equipment is: a thin film evaporator; the equipment in the water washing stage is as follows: a water washing tank; the equipment in the dehydration stage is as follows: a dehydrator; the equipment in the filtering stage is as follows: a filtering device and a finished product tank.
2. The system for preparing dibasic ester of adipic acid according to claim 1, wherein the reaction vessel has a raw material inlet on the side wall of the reaction section, a gas phase outlet on the top, a three-way valve on the gas phase outlet, and a reaction solution outlet on the bottom;
the condenser comprises a condensation inlet and a condensation outlet, and the condensation inlet is connected with the gas phase outlet through a three-way valve;
the water separator comprises a water separator inlet, a water separator first outlet and a water separator second outlet, wherein the water separator inlet is connected with the condensation outlet through a pipeline, and the water separator first outlet is connected with the gas phase outlet through a three-way valve.
3. The system for preparing dibasic adipate as claimed in claim 1, wherein the distillation kettle comprises a distillation kettle inlet connected with the second outlet of the water separator through a pipeline, an organic matter outlet at the top of the distillation kettle and a first wastewater outlet at the bottom of the distillation kettle.
4. The system according to claim 1, wherein the dealcoholization tower comprises a reaction solution inlet, a waste alcohol outlet and a crude product outlet, and the reaction solution inlet is connected to the reaction solution outlet through a pipeline.
5. The system for preparing adipic acid dibasic ester according to claim 1, wherein the thin film evaporator comprises a crude product inlet, a light component outlet and a heavy component outlet, and the crude product inlet is connected with the crude product outlet through a pipeline.
6. The system for preparing the dibasic ester of adipic acid as claimed in claim 1, wherein the water washing tank comprises a light component inlet, a water inlet and an upper product outlet, and the light component inlet and the light component outlet are connected through a pipeline.
7. The system of claim 1, wherein the dehydrator comprises an upper product inlet, a second wastewater outlet, and a material outlet, and the upper product inlet is connected to the upper product outlet through a pipeline.
8. The system for preparing adipic acid dibasic ester according to claim 1, wherein the inlet of the filtering device is connected with the material outlet, and the outlet of the filtering device is connected with a finished product tank through a pipeline.
CN201922387872.9U 2019-12-26 2019-12-26 Preparation system of adipic acid dibasic ester Active CN211170524U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Application Number Priority Date Filing Date Title
CN201922387872.9U CN211170524U (en) 2019-12-26 2019-12-26 Preparation system of adipic acid dibasic ester

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112387226A (en) * 2020-11-11 2021-02-23 润泰化学(泰兴)有限公司 Dealcoholization tower for producing isobutyl 2,2, 4-trimethyl-3-hydroxypentanoate
CN113045421A (en) * 2019-12-26 2021-06-29 江苏怡达化学股份有限公司 Preparation process and equipment of diisopropyl adipate
CN113045412A (en) * 2019-12-26 2021-06-29 江苏怡达化学股份有限公司 Preparation process and equipment of adipic acid dibasic ester

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113045421A (en) * 2019-12-26 2021-06-29 江苏怡达化学股份有限公司 Preparation process and equipment of diisopropyl adipate
CN113045412A (en) * 2019-12-26 2021-06-29 江苏怡达化学股份有限公司 Preparation process and equipment of adipic acid dibasic ester
CN112387226A (en) * 2020-11-11 2021-02-23 润泰化学(泰兴)有限公司 Dealcoholization tower for producing isobutyl 2,2, 4-trimethyl-3-hydroxypentanoate

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