Refining method for long-chain binary acid

A long-chain dibasic acid and refining method technology, which is applied in the field of long-chain dibasic acid refining, can solve the problems of high content of protein and other impurities, failure to meet the requirements of polymer grade products, and uneven crystal particle size, so as to save drying costs. Steam consumption, easy washing and filtering, coarse and uniform crystals

Active Publication Date: 2012-01-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, the use of the solvent method is greatly restricted due to large equipment investment, high production cost, residual solvents in the product, environmental pollution and safety issues.
Although the aqueous phase method overcomes the defects of the solvent method, the product has low purity, poor color, uneven crystal particle size, high content of protein and other impurities, and cannot meet the requirements of polymer grade products.
For example, CN95116450.3 discloses a method for treating α, ω dibasic acid fermentation broth, heating the terminated fermentation broth to remove unreacted alkanes, adding perlite, degerming by microfiltration, acidifying and crystallizing the filtrate, and drying Obtain dibasic acid, because this method does not carry out decolorization, product purity is low, and color and luster is poor
CN1611478A proposes a method for refining long-chain dibasic acids, which uses the combination of single salt crystallization and salting out, and terminates the fermentation broth through three times of alkali dissolution and multiple crystallization. The process is long, cumbersome, difficult to recover salt, and product yield low rate

Method used

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  • Refining method for long-chain binary acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1: Purify long-chain dibasic acid according to the following steps

[0019] Step 1: The pH of the fermented liquid produced by microbial fermentation to produce dodecanedibasic acid is adjusted to 8.5, heated to 60°C to break the emulsion, and filtered through a ceramic membrane to remove alkanes, bacteria, other macromolecular proteins, and pigment impurities to obtain a clear liquid;

[0020] Step 2: Add pure water to the clear liquid obtained in step 1 to adjust the salinity to 8%, add 0.1% activated carbon of the clear liquid mass for decolorization for 30 minutes, plate and frame press filter and wash the filter cake, dilute the decolorized clear liquid with pure water to control the salinity 4%;

[0021] Step 3: 6000ml of the decolorized clear liquid obtained in step 2 and dilute sulfuric acid with a mass concentration of 30% are subjected to rapid mixing and reaction crystallization on the molecular scale through a T-shaped microchannel reactor to form...

Embodiment 2

[0025] Embodiment 2: Purify long-chain dibasic acid according to the following steps

[0026] Step 1: adjust the pH of the fermented liquid to 8.8 after microbial fermentation to produce tridecanedibasic acid, heat to 75°C to break the emulsion, and filter through a ceramic membrane to remove alkanes, bacteria, other macromolecular proteins, and pigment impurities to obtain a clear liquid;

[0027] Step 2: Adjust the salinity of the clear liquid obtained in step 1 to 10%, add 0.3% activated carbon of the clear liquid mass for decolorization for 30 minutes, plate and frame press filter and wash the filter cake, dilute the decolorized clear liquid with steam condensate, and control the salinity to 5 %;

[0028] Step 3: 6000ml of the decolorized clear liquid obtained in step 2 and dilute sulfuric acid with a mass concentration of 40% are passed through a Y-type microchannel reactor for rapid mixing and reaction crystallization on the molecular scale to form a homogeneous mixture ...

Embodiment 3

[0032] Embodiment 3: Purify long-chain dibasic acid according to the following steps

[0033] Step 1: adjust the pH of the fermented liquid produced by microbial fermentation to tetradecanedibasic acid to 9.0, heat to 90°C to break the emulsion, and filter through a ceramic membrane to remove alkanes, bacteria, other macromolecular proteins, and pigment impurities to obtain a clear liquid;

[0034] Step 2: adjust the salinity of the supernatant obtained in step 1 to 12%, add 0.5% of the mass of the supernatant to decolorize with activated carbon for 30 minutes, plate and frame press filter and wash the filter cake, dilute the decolorized supernatant with purified water, and control the salinity to 6% ;

[0035] Step 3: 6000ml of the decolorized clear liquid obtained in step 2 and dilute sulfuric acid with a mass concentration of 50% are subjected to rapid mixing and reaction crystallization on the molecular scale through a T-shaped microchannel reactor to form a homogeneous mi...

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Abstract

The invention discloses a refining method for long-chain binary acid. The refining method comprises the steps of: performing pretreatments including demulsifying, filtering and decoloring on fermentation liquor, then, reacting the pretreated fermentation liquor with dilute sulphuric acid through a microchannel reactor, heating an obtained mixture by using a sleeve to remove fine crystals, introducing crystal mush into a crystallization kettle for curing, controlling the growing speed and the size of crystals by means of gradient temperature to form crystals with uniform particle size, filtering, washing and drying to obtain long-chain binary acid crystals. The long-chain binary acid crystals have the advantages of uniform particles, low content of protein and impurities, high product purity, good color, and capability of meeting requirements on quality of polymerization-level products.

Description

technical field [0001] The invention relates to a refining method, in particular to a refining method of a long-chain dibasic acid. Background technique [0002] The production of long-chain dibasic acids by microbial fermentation is a complex four-phase system, which contains unreacted normal alkanes, bacterial cells and debris, unused medium and metabolites, especially a large amount of impurities such as proteins and pigments , bringing great difficulty to the purification and refining of products. [0003] At present, the methods for refining long-chain dibasic acids are generally divided into two categories: solvent method and aqueous phase method. Among them, the use of the solvent method is greatly restricted due to large equipment investment, high production cost, residual solvent in the product, environmental pollution and safety issues. Although the aqueous phase method overcomes the defects of the solvent method, its product has low purity, poor color, uneven cr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/02C07C55/21C07C51/43
Inventor 桂秋芬邓怀林洪军业卢利玲蒋洋松沈旭
Owner CHINA PETROLEUM & CHEM CORP
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