Long-chain dicarboxylic acid with centralized granularity distribution and preparation method thereof

A long-chain dibasic acid and particle size distribution technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problem of concern about the particle size of long-chain dibasic acid separation and purification products

Active Publication Date: 2020-08-28
CATHAY R&D CENT CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far little attention has been paid to the particle size of long-chain dibasic acid separation and purification products

Method used

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  • Long-chain dicarboxylic acid with centralized granularity distribution and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0089] Dodecane dibasic acid crude product (purity is 95%) is placed in the decolorization tank, adds the activated carbon of 3.5% of dodecane dibasic acid crude product quality, and content is 95wt.% acetic acid, and this 95wt.% acetic acid conversion content is The mass ratio of 100wt.% acetic acid to the crude product of dodecanedibasic acid is 3:1, then decolorize at 80°C for 20min, and filter to obtain the dodecanedibasic acid solution. In the crystallizer, keep the dodecane dibasic acid solution at a constant temperature of 80°C for 1h.

[0090] The temperature was lowered to 60°C at a rate of 2min / °C. Particles were precipitated in the solution and the number of particles continued to increase. Raise the temperature to 67°C at a rate of 3min / °C, the number of particles in the solution decreases continuously, and the first temperature cycle ends; the second temperature cycle cools down to 52°C at a rate of 2min / °C, and then raises the temperature to 59°C at a rate of 3mi...

Embodiment 2

[0106] Dodecane dibasic acid (purity is 99%) and content is that 98wt.% acetic acid is placed in the crystallizer, and this 98wt.% acetic acid is converted into content and is after the acetic acid of 100wt.% and dodecane dibasic acid (purity is 99%) with a mass ratio of 2.2:1, heated to 85° C. to obtain a dodecanedioic acid solution.

[0107] In the crystallizer, keep the dodecanedibasic acid solution at a constant temperature of 85°C for 1h. Cooling down to 60°C at a rate of 2min / °C, particles precipitated in the solution and the number of particles continued to increase. Then the temperature was raised to 67°C at a rate of 3min / °C, the number of particles in the solution continued to decrease, and the first temperature cycle ended; the second temperature cycle was cooled to 52°C at a rate of 2min / °C, and then heated to 59°C at a rate of 3min / °C ℃,; for the third temperature cycle, cool down to 44°C at a rate of 2 min / °C, then raise the temperature to 51°C at a rate of 3 mi...

Embodiment 3

[0123] Undecane dibasic acid (purity is 99.1%) and content is that 95wt.% acetic acid is placed in the crystallizer, and this 95wt.% acetic acid is converted into the content after being 100wt.% acetic acid and purity is 99.1% The mass ratio of the basic acid is 2.8:1, heated to 80°C to obtain an undecanedibasic acid solution, and kept at a constant temperature of 80°C for 1 hour. Cool down to 55°C at a rate of 3min / °C, and keep at this temperature for 10min. Particles are precipitated in the solution and the number of particles continues to increase. Raise the temperature to 60°C at a rate of 5min / °C, keep at this temperature for 10min, the number of particles in the solution decreases continuously, and the first temperature cycle ends; the second temperature cycle cools down to 50°C at a rate of 3min / °C, at this temperature Keep warm for 10 minutes, heat up to 55°C at a rate of 5min / °C, and hold at this temperature for 10 minutes; for the third temperature cycle, cool down t...

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Abstract

The invention provides a method for controlling the granularity of long-chain dicarboxylic acid and the long-chain dicarboxylic acid with centralized granularity distribution prepared by the method. By using the method, the particle uniformity of the long-chain dicarboxylic acid product is improved, fine particles are few, the trouble of subsequent re-granulation of the product is avoided while the product quality is improved, the production cost is saved, the time is saved, the efficiency is high, and the method is suitable for industrial application.

Description

technical field [0001] The invention belongs to the technical field of industrial crystallization, and in particular relates to a long-chain dibasic acid with concentrated particle size distribution and a preparation method thereof. Background technique [0002] Long-chain dibasic acid refers to a straight-chain aliphatic dibasic acid with more than 10 carbon atoms in the carbon chain. It is the basic monomer material for a series of special synthetic materials, and can be used to produce special nylon, polycarbonate, powder coatings, and spices. , hot melt adhesives and special lubricants, etc. It is an important raw material for synthetic spices, engineering plastics, cold-resistant plasticizers, high-grade lubricants and polyamide hot melt adhesives, powder coatings and other products. [0003] Long-chain dibasic acids do not exist in nature, and some types of long-chain dibasic acids, such as sebacic acid and dodecanedioic acid, can be synthesized chemically. In additio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43C07C55/21C07C55/02
CPCC07C51/43C07C55/21C07C55/02
Inventor 董华杨晨秦兵兵刘修才
Owner CATHAY R&D CENT CO LTD
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