CN216571619U - 1, 5-pentanediamine moisture removal system for phosgenation reaction - Google Patents

1, 5-pentanediamine moisture removal system for phosgenation reaction Download PDF

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Publication number
CN216571619U
CN216571619U CN202123030547.0U CN202123030547U CN216571619U CN 216571619 U CN216571619 U CN 216571619U CN 202123030547 U CN202123030547 U CN 202123030547U CN 216571619 U CN216571619 U CN 216571619U
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pipe
dehydration tower
condenser
pentanediamine
moisture
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CN202123030547.0U
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Inventor
刘耀宗
王进军
李晓明
李卫俊
滕志君
杨英朝
陶春霞
陈�光
李虎邦
朱奕臻
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Gansu Yinguang Juyin Chemical Industry Co Ltd
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Gansu Yinguang Juyin Chemical Industry Co Ltd
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Abstract

The utility model relates to a 1, 5-pentanediamine moisture removal system for a phosgenation reaction, which is characterized in that: a gas phase pipe at the top of a distillation still (1) is connected into an inlet at the lower part of a dehydration tower (2), an exhaust pipe at the top of the dehydration tower (2) is connected into a condenser (3), a non-condensed gas exhaust pipe of the condenser (3) is connected into a vacuum system, a liquid outlet pipe at the bottom of the condenser (3) is connected into a water distributor (4), a reflux pipe at the lower part of the water distributor (4) is connected into the dehydration tower (2), and a liquid phase pipe at the bottom of the dehydration tower (2) is connected into the distillation still (1). Through the dehydration system, the moisture in the mixed solution can be reduced to be below 100 ppm, the corrosion of the moisture to the system is effectively reduced, the generation amount of three wastes is reduced, the operation process is simple, and the dehydration system is suitable for industrial production.

Description

1, 5-pentanediamine moisture removal system for phosgenation reaction
Technical Field
The utility model belongs to the field of chemical engineering technical equipment, and particularly relates to a 1, 5-pentanediamine moisture removal system for a phosgenation reaction.
Background
1, 5-Pentamethylene Diisocyanate (PDI) is novel aliphatic isocyanate, has yellowing resistance, is used for manufacturing the fields of yellowing-resistant polyurethane paint, ink and artificial leather in the forms of biuret and trimer, and has extremely wide market and application prospect. The raw material 1, 5-Pentanediamine (PDA) is basically prepared by a biological method, is influenced by the production process, has higher water content (more than 2000 ppm), is mainly aimed at industries such as nylon 5X and the like in a ten-thousand-ton PDA production device put into production at home at present, has low requirement on water content, and meets the requirement of the production process.
The phosgenation production process has high requirement on the water content in the raw materials, and the main reason is that the water content and the product hydrogen chloride in the reaction system can form hydrochloric acid to corrode equipment and pipelines, thereby causing potential safety hazards and increasing side reactions, so that the water content in the 1, 5-pentanediamine must be removed. In the traditional rectification process, due to the strong affinity effect of the 1, 5-pentanediamine and water, the water is difficult to effectively remove, and the deterioration of the 1, 5-pentanediamine is caused by high temperature, so that the development of a 1, 5-pentanediamine water removal system for the phosgenation reaction is urgently needed, the water content of raw materials is reduced, and the safe production is realized.
Disclosure of Invention
The utility model aims to remove moisture in the bio-based 1, 5-pentanediamine for the phosgenation reaction, avoid the corrosion of the moisture to a system, eliminate potential safety hazards and reduce the generation amount of three wastes.
In order to achieve the purpose, the utility model adopts the technical scheme that: the utility model provides a 1, 5-pentanediamine moisture desorption system for phosgenation reaction, includes stills, dehydration tower, condenser, water knockout drum, its characterized in that: the gas phase pipe at the top of the distillation still is connected to an inlet at the lower part of the dehydration tower, the exhaust pipe at the top of the dehydration tower is connected to a condenser, an exhaust pipe of non-condensed gas of the condenser is connected to a vacuum system, a liquid outlet pipe at the bottom of the condenser is connected to a water separator for keeping the negative pressure of the system, a reflux pipe at the lower part of the water separator is connected to the dehydration tower, and a liquid phase pipe at the bottom of the dehydration tower is connected to the distillation still. The upper part of the water separator is connected with a drain pipe L1 for removing the water in the system.
The principle of the utility model is as follows: by utilizing the azeotropic distillation and separation principle and adopting a distillation kettle and a dehydration tower, the water in the mixed material and the ortho-dichlorobenzene serving as a photochemical reaction solvent are evaporated, cooled and enter a water separator, the water is separated from the system by utilizing the density difference of the ortho-dichlorobenzene and water, and the ortho-dichlorobenzene returns to the distillation kettle, so that the continuous operation is realized.
The azeotropic distillation is to use ortho-dichlorobenzene as an entrainer, the solvent of photochemical reaction, to raise the ortho-dichlorobenzene and water to the top of a dehydration tower under the condition of negative pressure, to realize the separation of the 1, 5-pentanediamine from the water by controlling the process conditions such as reflux quantity and the like, and to prevent the 1, 5-pentanediamine from being decomposed at high temperature by controlling the temperature in a distillation kettle to be not more than 130 ℃.
The utility model has the beneficial effects that: the azeotropic distillation dehydration process is mature, the operation is simple, the water content of the mixed solution of the 1, 5-pentanediamine and the o-dichlorobenzene can be effectively reduced to be less than 100 ppm, and the control index of the photochemical reaction raw materials is achieved. The dehydrated mixed solution can be directly used for phosgenation production, simplifies the process flow, avoids the corrosion of moisture to the pipeline of the phosgenation system equipment, reduces the three wastes generated by the reaction of the moisture and the product, is suitable for industrial production, and has strong practicability and popularization in the same industry.
Drawings
FIG. 1 is a schematic view of the present invention;
in the figure: 1-distillation still, 2-dehydration tower, 3-condenser, 4-water knockout drum.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the utility model.
Example 1, referring to fig. 1, a 1, 5-pentanediamine moisture removal system for phosgenation reaction, comprising a distillation still 1, a dehydration tower 2, a condenser 3 and a water separator 4, wherein: under the negative pressure condition, a gas phase pipe at the top of the distillation still 1 is connected to an inlet at the lower part of the dehydration tower 2, an exhaust pipe at the top of the dehydration tower 2 is connected to the condenser 3, an exhaust pipe of the non-condensed gas of the condenser 3 is connected to the vacuum system, a liquid outlet pipe at the bottom of the condenser 3 is connected to the water separator 4, a return pipe at the lower part of the water separator 4 is connected to the dehydration tower 2, and a liquid phase pipe at the bottom of the dehydration tower 2 is connected to the distillation still 1.
The condenser 3 is connected with a circulating water inlet pipe and a circulating water outlet pipe and used for cooling materials.
The distillation still 1 is connected with medium-pressure steam and condensate pipelines and used for heating materials.
The water separator 4 is connected with a drain pipe and used for removing system moisture.
The working process is as follows: the method comprises the following steps of enabling mixed steam of 1, 5-pentanediamine and o-dichlorobenzene containing moisture to enter a dehydration tower 2 through a gas phase pipe at the top of a distillation kettle 1, filling pall ring fillers in the dehydration tower 2, enabling a liquid phase in the tower to return to the distillation kettle 1 through a liquid phase pipe, enabling a gas phase to enter a condenser 3 through an exhaust pipe, enabling non-condensable gas of the condenser 3 to enter a vacuum system, enabling condensate to enter a water separator 4, enabling a water phase and an organic phase to be separated in the water separator 4, enabling the upper-layer water phase to be discharged and recycled, enabling the lower-layer organic phase to enter the dehydration tower 2 through a backflow pipe and return to the distillation kettle 1, continuously operating, and sampling and analyzing the qualified moisture content to be used for a phosgenation reaction.

Claims (2)

1. The utility model provides a 1, 5-pentanediamine moisture desorption system for phosgenation reaction, includes stills (1), dehydration tower (2), condenser (3), water knockout drum (4), its characterized in that: a gas phase pipe at the top of a distillation kettle (1) is connected into an inlet at the lower part of a dehydration tower (2), an exhaust pipe at the top of the dehydration tower (2) is connected into a condenser (3), a non-condensed gas discharge pipe of the condenser (3) is connected into a vacuum system, a liquid outlet pipe at the bottom of the condenser (3) is connected into a water distributor (4), a return pipe at the lower part of the water distributor (4) is connected into the dehydration tower (2), and a liquid phase pipe at the bottom of the dehydration tower (2) is connected into the distillation kettle (1).
2. A moisture removal system for 1, 5-pentanediamine used in the phosgenation reaction of claim 1, wherein: the upper part of the water separator (4) is connected with a drainage pipe L1.
CN202123030547.0U 2021-12-06 2021-12-06 1, 5-pentanediamine moisture removal system for phosgenation reaction Active CN216571619U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202123030547.0U CN216571619U (en) 2021-12-06 2021-12-06 1, 5-pentanediamine moisture removal system for phosgenation reaction

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202123030547.0U CN216571619U (en) 2021-12-06 2021-12-06 1, 5-pentanediamine moisture removal system for phosgenation reaction

Publications (1)

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CN216571619U true CN216571619U (en) 2022-05-24

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4375269A1 (en) 2022-11-24 2024-05-29 Covestro Deutschland AG Method for drying 1,5-diaminopentane

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4375269A1 (en) 2022-11-24 2024-05-29 Covestro Deutschland AG Method for drying 1,5-diaminopentane
WO2024110339A1 (en) 2022-11-24 2024-05-30 Covestro Deutschland Ag Process for drying 1,5-diaminopentane

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