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Method and device for separating, refining and purifying intermediate m-xylylene dicarbamate solution and application of intermediate m-xylylene dicarbamate solution

A technology of ethyl isoxylylene dicarbamate and solution, which is applied in the field of separation, purification and purification of ethyl isoxylylene dicarbamate solution of an intermediate, and can solve the problems of unmentioned methods of separation and purification, Influence and other problems, to achieve the effect of efficient recycling and improving product quality

Active Publication Date: 2022-05-13
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] CN110467546A discloses a method for preparing m-xylylene diisocyanate, the method comprising: dissolving ethyl m-xylylene dicarbamate in an organic solvent, carrying out a thermal decomposition reaction under protective gas purging, The m-xylylene diisocyanate is obtained, but the method for the separation and purification of the intermediate m-xylylene dicarbamate (XDC) is not mentioned, and the purity of the intermediate has an important impact on the quality of the isocyanate

Method used

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  • Method and device for separating, refining and purifying intermediate m-xylylene dicarbamate solution and application of intermediate m-xylylene dicarbamate solution
  • Method and device for separating, refining and purifying intermediate m-xylylene dicarbamate solution and application of intermediate m-xylylene dicarbamate solution
  • Method and device for separating, refining and purifying intermediate m-xylylene dicarbamate solution and application of intermediate m-xylylene dicarbamate solution

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Embodiment 1

[0055] This embodiment provides a method for the separation, purification and purification of the intermediate m-xylylenedicarbamate solution, and the schematic flow chart of the method is as follows figure 1 As shown, the method includes the following steps:

[0056] Provide XDC solution synthesized under high temperature and high pressure (3.2MPa, 200°C), the main components in the XDC solution include intermediate m-xylylene dicarbamate, solvent ethanol, carbonylating agent ethyl carbamate And trace impurities and by-products.

[0057] (1) Send the XDC solution to the flash tank 1 for flash evaporation at 0.2 MPa, separate part of the solvent ethanol at the top, and obtain the first concentrated solution of XDC whose temperature drops to 110°C at the bottom;

[0058] (2) Transfer the first concentrate of XDC obtained in step (1) to the solvent separation tower 2 for the first rectification (the pressure is 30kPa, the temperature of the tower is 120°C), the remaining solven...

Embodiment 2

[0068] This embodiment provides a method for the separation, purification and purification of the intermediate m-xylylenedicarbamate solution, the method comprising the following steps:

[0069] Provide XDC solution synthesized under high temperature and high pressure (3.6MPa, 210°C), the main components in the XDC solution include intermediate m-xylylene dicarbamate, solvent ethanol, carbonylating agent ethyl carbamate And trace impurities and by-products.

[0070] (1) Send the XDC solution to the flash tank 1 for flash evaporation at 0.1 MPa, separate part of the solvent ethanol at the top, and obtain the first concentrated solution of XDC whose temperature drops to 85°C at the bottom;

[0071] (2) Transfer the first concentrate of XDC obtained in step (1) to the solvent separation tower 2 for the first rectification (the pressure is 50kPa, the temperature of the tower bottom is 130°C), the remaining solvent ethanol is separated at the top of the tower, and XDC is obtained a...

Embodiment 3

[0081] This embodiment provides a method for the separation, purification and purification of the intermediate m-xylylenedicarbamate solution, the method comprising the following steps:

[0082] Provide XDC solution synthesized under high temperature and high pressure (1.7MPa, 180°C), the main components in the XDC solution include intermediate m-xylylene dicarbamate, diethyl carbonate, ethanol and trace impurities and by-product.

[0083] (1) Send the XDC solution to the flash tank 1 for flash evaporation at 0.15 MPa, separate part of the solvent ethanol at the top, and obtain the first concentrated XDC solution whose temperature drops to 110°C at the bottom;

[0084] (2) Transfer the first concentrate of XDC obtained in step (1) to the solvent separation tower 2 for the first rectification (the pressure is 80kPa, the temperature of the tower bottom is 90°C), the remaining solvent ethanol is separated at the top of the tower, and XDC is obtained at the bottom of the tower se...

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Abstract

The invention provides a method and a device for separating, refining and purifying an intermediate ethyl m-xylylene dicarbamate solution and application of the intermediate ethyl m-xylylene dicarbamate solution. The method comprises the following steps: sequentially carrying out flash evaporation, first rectification and second rectification on an XDC solution, carrying out first-stage washing, first-stage oil-water separation, first-stage evaporation, second-stage evaporation, second-stage washing, second-stage oil-water separation and dehydration treatment to obtain refined and purified XDC; according to the method, a series of separation processes are designed according to the properties of the XDC and impurities contained in the solution, so that the separation, refining and purification of the XDC can be safely and stably realized, the impurities in the XDC solution are thoroughly removed, the residual quantity of impurity ions and metal oxides in the product is less than 10ppm, and the product quality is improved; the method can also efficiently recover the carbonylation agent and the solvent for cyclic utilization, has certain economical efficiency, and is beneficial to industrial application.

Description

technical field [0001] The invention belongs to the technical field of compound separation and purification, and in particular relates to a method, device and application for separation, purification and purification of an intermediate m-xylylene diurethane solution. Background technique [0002] Isocyanate is a special chemical with isocyanate (N=C=O) functional group, and is an important raw material for the production of polyurethane products. M-xylylene diisocyanate (XDI) belongs to aliphatic diisocyanate. XDI introduces methylene between the benzene ring and the isocyanate group, which prevents the influence of the benzene ring macromolecular conjugation effect on the –NCO group, making it The isocyanate group of XDI is inherently more stable, so its properties are close to those of aliphatic isocyanates. Compared with hexamethylene diisocyanate (HDI), isophorone diisocyanate (IPDI) and p-phenylene diisocyanate (PPDI), XDI has better addition reactivity, and its adhesi...

Claims

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Application Information

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IPC IPC(8): C07C269/08C07C271/20C07C263/04C07C265/14
CPCC07C269/08C07C263/04C07C271/20C07C265/14
Inventor 王利国陈家强曹妍李会泉贺鹏郑征徐爽齐世锋王宜飞孟凡军冯海猛
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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