Refining and purifying method of long carbon chain dicarboxylic acid

A technology of long-chain dibasic acid and dibasic carboxylic acid, which is applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc. The purification yield of chain dibasic acid, the difficulty of removing impurities, etc., are beneficial to environmental protection, avoid the problem of heterogeneous nucleation, and save raw materials and water resources.

Inactive Publication Date: 2018-05-08
ZIBO GUANGTONG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The removal of impurities increases the difficulty
Simultaneously, also reduced the purification yield of long carbon chain dibasic acid
[0014] 2. Cooling natural crystallization method, the crystallization mother liquor remaining in the decolorized filter cake has not been replaced, that is, washing with high temperature water, when a large amount of water contacts the crystallization mother liquor remaining in the filter cake, due to the influence of water on the solubility of acetic acid , so that the dissolved impurities in the mother liquor are precipitated instantly, and the residues in the filter cake are difficult...

Method used

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  • Refining and purifying method of long carbon chain dicarboxylic acid
  • Refining and purifying method of long carbon chain dicarboxylic acid
  • Refining and purifying method of long carbon chain dicarboxylic acid

Examples

Experimental program
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Effect test

Embodiment 1

[0121] A kind of refining purification method of dodecanedioic acid of the present invention

[0122] In a 3000L dissolving and decolorizing reaction kettle, put 2000L of 98% acetic acid solution, 800kg of crude dodecanedioic acid, and 6kg of activated carbon, stir well, heat up to 95°C, keep warm for 20 minutes, pass through an underflow plate and frame filter press, bag type The dodecanedioic acid solution filtered by the filter, metal titanium rod filter, and laminated filter four-stage filtration system enters the crystallization kettle, and quickly and uniformly cools down to 78°C in the crystallization kettle, turns off the cooling water, and naturally cools down to 75°C , add dodecanedioic acid with a purity greater than 99.8% as a seed crystal, control the stirring speed at 40r / min, the temperature in the crystallization tank rebounds to 77°C, and then gradually decreases, when the temperature naturally drops to 68°C, slowly turn on the cooling water , control the cool...

Embodiment 2

[0125] A kind of refining purification method of dodecanedioic acid of the present invention

[0126] In a 3000L dissolving and decolorizing reactor, drop into 1800L of 98% acetic acid solution, 760kg of dodecanedioic acid crude product, 6kg of gac, and 200L of acetic acid rinse filtrate obtained in Example 1 was stirred evenly, heated to 95°C, kept for 20 minutes, and heated to 95°C for 20 minutes. Underflow plate and frame filter press, bag filter, metal titanium rod filter, laminated filter four-stage filtration system, the dodecanedioic acid solution obtained by filtration enters the crystallization kettle, and quickly and uniformly cools down to 77°C in the crystallization kettle , turn off the cooling water, naturally cool down to 73°C, add dodecanedioic acid with a purity greater than 99.8% as a seed crystal, control the stirring speed at 40r / min, the temperature in the crystallization tank rebounds to 75°C, and then gradually drops, the temperature naturally When it dr...

Embodiment 3

[0129] A kind of refining purification method of tetradecanedioic acid of the present invention

[0130] In a 3000L dissolving and decolorizing reaction kettle, put 2000L of 98% acetic acid solution, 660kg of crude tetradecanedioic acid, and 6kg of activated carbon, stir well, heat up to 95°C, keep warm for 20 minutes, and pass through an underflow plate and frame filter press, bag type The tetradecanedioic acid solution filtered by the filter, metal titanium rod filter, and laminated filter four-stage filtration system enters the crystallization kettle, and the temperature is quickly and uniformly cooled to 78°C in the crystallization kettle, and the cooling water is turned off, and the temperature is naturally cooled to 75°C , add tetradecanedioic acid with a purity greater than 99.8% as a seed crystal, control the stirring speed to 40r / min, the temperature in the crystallization tank rebounds to 77°C, and then gradually decreases, when the temperature naturally drops to 68°C...

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Abstract

The invention provides a refining and purifying method of long carbon chain dicarboxylic acid. The refining and purifying method is characterized in that the raw material moisture content of a long chain binary acid coarse product is controlled to be smaller than or equal to 1.0 wt%; the content of solvent acetic acid is larger than or equal to 95.0 wt%; the crystallization process adopts three-section gradient cooling, and induction seed crystal is added after second-section cooling to induce crystallization; crystalized filter cake is firstly sprayed by acetic acid, is next washed by water and is then subjected to centrifugal filtering; then the filter cake is washed by the water at environment temperature; an acetic acid solvent generated in the refining process is totally recycled through an azeotropic distillation method; a cleaning solution and a mother solution which are generated in the refining process are totally recycled. The refining and purifying method, high in product yield, low in refining cost and high in purity, of long carbon chain dicarboxylic acid is provided. The total acid content of long carbon chain dicarboxylic acid after being refined and purified reaches99.90%, the single acid content reaches 99.45%, the total nitrogen content reaches 6ppm, the ferric ion content reaches 0.5 ppm, the ash content is smaller than or equal to 10 ppm, and the moisture content is smaller than or equal to 0.16%. The purifying comprehensive yield reaches 98.64%. All quality technical indexes meet a user's requirements.

Description

technical field [0001] The invention is a refining and purifying method of long carbon chain dicarboxylic acid. It belongs to the purification treatment of acyclic dicarboxylic acids with more than 10 carbon atoms. Background technique [0002] Long-chain dicarboxylic acid (along-chain dicarboxylic acid)—a straight-chain dicarboxylic acid with more than 10 carbon atoms in the carbon chain, is an important class of fine chemical products. Main raw materials for synthesizing polyamide resins, polyester resins, hot melt adhesives, spices, weather-resistant plasticizers, lubricating oil additives, coatings, liquid crystals, etc. [0003] The main industrial applications include artificial synthesis of muscone; coil adhesives used for a long time at 100°C; hot-melt adhesives for clothing setting; not only can manufacture high-temperature resistant lubricants, but also can manufacture effective at -45°C low temperature Lubricating lubricant; high-performance coatings made of lon...

Claims

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Application Information

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IPC IPC(8): C07C55/21C07C55/02C07C51/43
CPCC07C51/43C07C55/21C07C55/02
Inventor 房宁
Owner ZIBO GUANGTONG CHEM
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