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A method for separation and purification of durene based on bubble fractional crystallization and distillation

A technology of durene and fractional crystallization, which is applied in the directions of crystallization purification/separation, distillation purification/separation, chemical instruments and methods, etc., which can solve the problems of complex process route, poor production environment and low operability of the preparation method, Achieve the effect of improving efficiency and product purity, improving clearance rate and low energy consumption

Active Publication Date: 2020-10-20
连云港鹏辰特种新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] It can be known from the above-mentioned prior art that different yields and purities of durene can be obtained by purifying the distilled durene-enriched liquid through different crystallization methods, but the preparation method has complicated process routes, high energy consumption and operability. Low, low work efficiency, poor production environment, there is still a lot of room for improvement in the purity and yield of durene

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  • A method for separation and purification of durene based on bubble fractional crystallization and distillation

Examples

Experimental program
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Effect test

Embodiment 1

[0025] (1) The material containing 50% durene is added to the crystallizer, and small nitrogen bubbles with a flow rate of 40L / h are introduced from bottom to top, and the temperature is first lowered to -10°C, and then cooled to - at a rate of 0.5°C / min. 25°C, crystallization treatment for 50 minutes, nitrogen gas bubbles with a flow rate of 30L / h from top to bottom, and the crystallized crystals were filtered through a 56°C porous sieve attached to nano-scale metal particles at an angle of 45° for 5 minutes. The aperture of the sieve is 0.5-1mm, and the crude durene is obtained.

[0026] (2) After the crude durene is heated and melted at 130°C, small nitrogen bubbles with a flow rate of 15L / h are introduced from bottom to top, and the temperature is first raised to 190°C at a rate of 5°C / min, and then heated at a rate of 0.1°C / min. The rate of min continues to heat up to 196°C for heat preservation treatment, and the steam is condensed and recovered to obtain separated and p...

Embodiment 2

[0028] (1) The material containing 55% durene is added to the crystallizer, and small nitrogen bubbles with a flow rate of 60L / h are introduced from bottom to top, and the temperature is first lowered to -15°C, and then cooled to - at a rate of 1°C / min. 30°C, crystallization treatment for 90 minutes, nitrogen small bubbles with a flow rate of 50L / h from top to bottom, and the crystallized crystals were filtered through a porous sieve attached to nano-scale metal particles at 60°C for 50 minutes. The aperture of the sieve is 3-5 mm, and the crude durene is obtained.

[0029] (2) After the crude durene was heated and melted at 135°C, small nitrogen bubbles with a flow rate of 45L / h were introduced from bottom to top, and the temperature was first raised to 190°C at a rate of 10°C / min, and then heated at a rate of 0.5°C / min. The rate of min continues to heat up to 198°C for heat preservation treatment, and the steam is condensed and recovered to obtain separated and purified dure...

Embodiment 3

[0031] (1) The material containing 60% durene is added to the crystallizer, and small nitrogen bubbles with a flow rate of 55L / h are introduced from bottom to top, and the temperature is first lowered to -13°C, and then cooled to - at a rate of 0.7°C / min. 24°C, crystallization treatment for 60min, nitrogen gas bubbles with a flow rate of 35L / h from top to bottom, and the precipitated crystals were filtered through a porous sieve attached to nano-scale metal particles at 57°C for 30min, in which the porous The aperture of the sieve is 1-3mm, and the crude product of durene is obtained.

[0032] (2) After the crude durene is heated and melted at 132°C, small nitrogen bubbles with a flow rate of 20L / h are introduced from bottom to top, and the temperature is first raised to 190°C at a rate of 7°C / min, and then heated at a rate of 0.2°C / min. The rate of min continues to heat up to 197°C for heat preservation treatment, and the steam is condensed and recovered to obtain separated a...

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Abstract

The invention provides a durene separation and purification method based on stepped bubble crystallization and distillation. The method is characterized by comprising the following steps: adding a durene-containing material into a crystallizer, introducing small nitrogen bubbles from bottom to top, cooling to a temperature of 10-15 DEG C below zero, then cooling to a temperature of 25-30 DEG C below zero, performing crystallization treatment, introducing the small nitrogen bubbles from top to bottom, and filtering the crystallized and settled crystal through a tilting porous screen so as to obtain coarse durene; heating and melting the coarse durene, introducing the small nitrogen bubbles from bottom to top, raising the temperature to 190 DEG C, continuously raising the temperature to 196-198 DEG C, maintaining the temperature, and performing condensation recovery on steam, thereby obtaining the separated and purified durene. According to the method disclosed by the invention, crystallization and evaporation of the durene can be accelerated by utilizing a bubble technique, and along with an accurate temperature control technology, on the basis of reducing the energy consumption, the durene separation and purification efficiency can be obviously improved. The method is simple, high-efficiency, high in controllability and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of durene separation, in particular to a method for separating and purifying durene based on bubble fractional crystallization and distillation. Background technique [0002] Durene, that is, 1,2,4,5-tetramethylbenzene, has a symmetrical dipole pair. Its boiling point is 196.8°C and melting point is 79.2°C, which is higher than that of its isomers, tetramethylbenzene and partial tetramethylbenzene , camphor odor, white crystal, soluble in ether, ethanol and other organic solvents, insoluble in water, can sublime, its derived polymer has stepped alternating single bonds and double bonds, good high temperature resistance, therefore, the market demand increasing day by day. [0003] At present, durene can be obtained through synthesis reactions such as separation or isomerization from C10 aromatics. The traditional separation and purification technology is to first rectify and cut fractions with different boil...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C7/14C07C7/04C07C15/02
CPCC07C7/005C07C7/04C07C7/14C07C15/02
Inventor 谈勇谈俊江晓龙胡涛
Owner 连云港鹏辰特种新材料有限公司
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