Purification method of long-carbon-chain dicarboxylic acid

A long carbon chain dibasic acid and dibasic carboxylic acid technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problem of difficult to obtain polymers with a high degree of polymerization, affecting the mechanical properties of products, edible alcohol, etc. Problems such as high price, to achieve the effect of reducing coexistence time, low cost, and reducing the probability of side reactions of esterification

Active Publication Date: 2015-04-22
山东广通新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When polyamide is used as a raw material to produce polyamide products, short chains will be polymerized, and it is difficult to produce high-molecular polymers with high polymerization degree and regular molecular weight, which will affect the mechanical properties of the product.
And glacial acetic acid is extremely corrosive when the temperature exceeds 60°C. Even if expensive titanium equipment is used, the equipment cannot be completely prevented from being corroded.
[0014] 2. Most of the solvents used in

Method used

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  • Purification method of long-carbon-chain dicarboxylic acid
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  • Purification method of long-carbon-chain dicarboxylic acid

Examples

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Embodiment 1

[0110] A C of the present invention 12 Purification method of dicarboxylic acid

[0111] 600kgC 12 Dibasic carboxylic acid and 6kg of activated carbon are added to 2000L of methanol solution with a purity of 98%. After stirring evenly, the temperature of the plate heat exchanger is raised and it enters the decolorization kettle. The dibasic acid solution enters the crystallization kettle, quickly and uniformly cools down to 47°C in the crystallization kettle, controls the cooling time for 20 minutes, turns off the cooling water, and naturally cools down for 1 hour. ℃, control the cooling time for 3 hours. Centrifugal separation of the crystallization liquid, rinse the material in the centrifuge with 300L methanol solution with a purity of 98%, centrifuge for 15 minutes after the rinse, and obtain a material with a solid content of 84%, and dry it in a double-cone vacuum dryer to obtain a refined dibasic acid , the total acid content measured by neutralization titration is 9...

Embodiment 2

[0113] A C of the present invention 12 Purification method of dicarboxylic acid

[0114] 400kgC 12Dibasic carboxylic acid and 6 kg of activated carbon are added to 2000 L of centrifuged mother liquor (including washing liquid) obtained in Example 1. After stirring evenly, the temperature of the plate heat exchanger enters the decolorization kettle, and the material outlet temperature of the plate heat exchanger is controlled at 60-64 ° C. The dibasic acid solution filtered by the filtration system enters the crystallization kettle, and quickly and uniformly cools down to 47°C in the crystallization kettle, controls the cooling time for 20 minutes, turns off the cooling water, and naturally cools down for 1 hour. Cool down to 25°C evenly, and control the cooling time for 3 hours. The crystallization liquid is centrifuged, and the centrifuged material is mixed with 2000L methanol solution with a purity of 98% at 20°C in 3m 3 Stir in the enamel kettle for 20 minutes, and centr...

Embodiment 3

[0116] A C of the present invention 12 Purification method of dicarboxylic acid

[0117] 400kgC 12 Dibasic carboxylic acid and 4 kg of activated carbon were added to 2000 L of the washing liquid obtained in Example 2, stirred evenly, and then heated up through the plate heat exchanger and entered into the decolorization kettle. The dibasic acid solution enters the crystallization tank, quickly and uniformly cools down to 47°C in the crystallization tank, controls the cooling time for 20 minutes, turns off the cooling water, and naturally cools down for 1 hour, the temperature in the crystallization tank reaches 43.2°C, turns on the cooling water and evenly cools down to 25°C , control the cooling time for 3 hours. Centrifugal separation of the crystallization liquid, rinse the material in the centrifuge with 300L methanol solution with a purity of 98%, centrifuge for 15 minutes after the rinse, and obtain a material with a solid content of 83%, and dry it in a double-cone va...

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Abstract

The invention relates to a purification method of long-carbon-chain dicarboxylic acid, belonging to purification treatment of cycle-free dicarboxylic acid with more than 10 carbon atoms. The invention is characterized in that recrystallizing purification is performed by using a long-carbon-chain dibasic acid crude product produced by a microbial fermentation process as an initial raw material and methanol as a solvent. The method comprises the following steps: (1) dissolving and decolorizing: a. feeding at room temperature, b. dissolving by preheating, c. decolorizing by adsorption, and d. four-stage filtering; (2) gradient cooling and crystallization; (3) eluting and centrifugal filtration; and (4) vacuum drying. The technical indexes of the purified long-carbon-chain dicarboxylic acid are as follows: the single acid content is at least 90.20%, the total acid content is 99.60 wt%, the ash content is at most 30 ppm, the iron content on the basis of Fe2O3 is at most 2 ppm, the total nitrogen on the basis of N is at most 30 ppm, the moisture content is at most 0.4 wt%, and no ester content is detected. The purification yield of C11-C14 is greater than or equal to 98.4%. The long-carbon-chain dicarboxylic acid is suitable to be used as a polycondensation monomer to perform polycondensation reaction with diamine to synthesize the long-carbon-chain nylon, and is also suitable to be used as a raw material of synthetic perfume and drugs. The purification method of long-carbon-chain dicarboxylic acid has the advantages of favorable product color, high product purity, high refinement yield and lower cost.

Description

technical field [0001] The invention is a method for purifying long carbon chain dicarboxylic acids. 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] Use long-chain dicarboxylic acids as raw materials to develop plasticizers with excellent performance used in the production of PVC (polyvinyl chloride), such as long-chain dibasic acid dibutanol ester, dihexyl alcohol ester, dioctyl alcohol ester, etc. . Replace existing phthalic acid and aliphatic dibasic acid esters; develop long-chain dibasic acid d...

Claims

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Application Information

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IPC IPC(8): C07C51/42C07C51/47C07C51/43C07C55/21C07C55/02
CPCC07C51/42C07C51/43C07C51/47C07C55/21C07C55/02
Inventor 房宁郝本清张亮杨光耀
Owner 山东广通新材料有限公司
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