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Double-stage purification method of long chain dicarboxylic acid aqueous phase

A long-chain dibasic acid and purification method technology, which is applied in the field of long-chain dibasic acid aqueous phase two-stage purification, can solve the problems of low production cost, short process route, low purity, etc., to avoid cost increase and reduce residue , to avoid the effect of low product yield

Inactive Publication Date: 2014-01-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to: provide a long-chain dibasic acid water-phase two-stage purification method, so that its product index can meet the requirements of polymerization-grade product index, the process route is short, the production cost is low, the product yield is high, the purity is high, and it has good performance. The water-phase crystal form solves the shortcomings of the existing water-phase method, such as low purity, high protein content, and poor color, and is conducive to large-scale industrial production

Method used

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  • Double-stage purification method of long chain dicarboxylic acid aqueous phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Pure long chain binary acids according to the following steps

[0025] (1) Twelve carbon di -carbonic acid with a concentration of 160g / L and PH8.5 terminated the fermentation solution 95 ° C to heat the milk and breaks the milk.Membrane liquid layer;

[0026] (2) Dilute the microfiltrate membrane clearing fluid to 10%of the salinity value. Under the condition of weak alkaline pH9.0, heated to 100 ° C after adding a microfillet membrane amount of sodium hydrochloride, shielding dual acid acidCarboxyl group and reducing impurities reaction, after reaction;

[0027] (3) Stir heating steps (2) The long -chain binary acid clearing solution is treated to 100 ° C, and the acetic acid is adjusted to PH4.0 in the regional stable area;Long -chain dual acid filter cake layer, acid washing water recycling to be treated; after the saturated hydrochloric acid water in the dual acid filter cake, use pure water to further wash it twice to remove the sodium salt, dry, and get th...

Embodiment 2

[0028] Example 2: Pure long chain binary acids according to the following steps

[0029] (1) Thirteen carbon di -carbonic acid with a concentration of 160g / L, PH8.5 terminate the fermentation solution at 80 ° C to heat up milk, and use ceramic micro filter membrane to remove the unprecedented alkane, yeast, pigment macromolecules to obtain microfiltrationMembrane liquid layer;

[0030] (2) Dilute the microfiltrate membrane clearing fluid to the salinity value of 4%. Under the condition of weak alkaline pH7.8 conditions, after heating to 80 ° C, the amount of sodium hydrochloride of 2%oxide of the microfilment membrane liquid is shielded.Carboxyl group and reducing impurities reaction, after reaction;

[0031] (3) Stir heating steps (2) The long -chain binary acid clearing solution is treated to 80 ° C, and the sulfuric acid is adjusted to the pH 3.5 dispersing area;Washing long chain dual acid filter layer, acid washing water recycling is to be treated; after the saturated hydroch...

Embodiment 3

[0032] Example 3: Pure long chain binary acids according to the following steps

[0033] (1) Fifteen -carbon di -carbonic acid with a concentration of 160g / L and PH8.5 terminated the fermentation solution 90 ° C to heat up milk and breaks the milk and breaks out.Membrane liquid layer;

[0034] (2) Dilute the microfiltrate membrane clearing fluid to the salinity value of 7%. Under the condition of weak alkaline pH8.0, heated to 90 ° C after adding a microfilinal solution to 5%oxidant ozone, shielded dual acid acidCarboxyl group and reducing impurities reactions, reacting the backboard frame to filter out the liquid;

[0035] (3) Stir heating steps (2) The long -chain binary acid clearing solution is treated to 95 ° C, and the mixed acids of phosphate and bidine are adjusted to the pH5.0 dispersing area;Sodium carbonate acid washing water washing long -chain dual acid filter layer, acid washing water recycling is to be treated; after the saturated hydrochloric acid water in the dual...

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Abstract

The invention discloses a double-stage purification method of a long chain dicarboxylic acid aqueous phase. The double-stage purification method comprises the following steps: (1) heating and demulsifying terminated fermentation broth of long chain dicarboxylic acid produced by a fermentation method, and filtering the terminated fermentation broth through a ceramic microfiltration membrane to obtain a microfiltration membrane supernatant layer; (2) diluting the microfiltration membrane supernatant, and adding an oxidizing agent under a weak alkaline condition to react to obtain supernatant; or diluting the microfiltration membrane supernatant, and adding the oxidizing agent under a weak acidic condition to react to obtain the supernatant; or diluting the microfiltration membrane supernatant, filtering the microfiltration membrane supernatant through a microfiltration membrane, diluting, and adding the oxidizing agent to react to obtain the supernatant; (3) regulating the pH value of the supernatant to 3.0-5.0 through an acid, maintaining the temperature for 1 h, filter pressing through a plate frame, washing a long chain dicarboxylic acid filter cake layer through acidic washing water of a saturated sodium salt, press filtering the acidic water of saturated salt in the dicarboxylic acid filter cake, removing the sodium salt from the pure water, and drying to obtain a long chain dicarboxylic acid product. The double-stage purification method disclosed by the invention is short in process route, low in production cost, high in yield, high in purity, good in aqueous phase crystal morphology, capable of solving the defects of a current aqueous phase method product of low purity, high protein content and bad color and luster, and beneficial for large-scale industrial production.

Description

Technical field [0001] The present invention involves the method of water phase refinement in the process of long chain binary acids, and specifically involves dual -phase purification methods of long -chain binary acid water phase phase. Background technique [0002] C 11 -C 18 Straight alkane hydrocarbons are raw materials, and use tropical fake silk yeast cells to oxidize the bipolar carboxyl lines of bipoar carboxyl group.The conditions of biometification are mild, easy to crafts, and easy to obtain products, but the refining method of polymerization product is still limited to organic solvents refining technology. It has disadvantages such as heavy pollution and harsh operation environment.In the groping.This is because the fermentation system is a mixture of residual alkane, emulsifier, bacteria, medium and various metabolites.Due to the low solubility of long -chain binary acids in the water phase, the phenomenon of organic impurities such as clip pigment, nitrogen compoun...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/02C07C51/42C07C51/50C07C51/48
CPCC07C51/42C07C51/50C07C55/02
Inventor 姚嘉旻桂秋芬卢利玲
Owner CHINA PETROLEUM & CHEM CORP
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