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C12-C13 long-chain binary acid refining method

A C12-C13, 1.C12-C13 technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve the problems of difficult process control, environmental pollution, high cost, and achieve easy process control, solvent The effect of easy source and low equipment requirements

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

AI Technical Summary

Problems solved by technology

2. Preparation by chemical synthesis: All long-chain dibasic acids cannot be directly oxidized from n-alkanes in petroleum by chemical methods, because during chemical oxidation, n-alkanes undergo chain scission and cannot obtain n-alkanes A single dibasic acid with a corresponding chain length. So far, only dodecane dibasic acid can be synthesized by chemical methods for industrial production. It uses butadiene as a raw material and is synthesized through 9 complicated reaction steps. It requires both High temperature, high pressure and catalysts require fireproof, explosion-proof and poison-proof devices. Due to harsh conditions, many steps, low yield, high cost and serious environmental pollution, it affects its large-scale industrial production
However, due to the difficulty in controlling the process of generating mono-salt, cumbersome operation steps and the disadvantages of low mono-acid content and low yield, it is difficult to be popularized and applied industrially.

Method used

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  • C12-C13 long-chain binary acid refining method

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Example 1: Add 10g of crude dodecanedibasic acid and 1g of activated carbon with an average particle size of 300 mesh into a pressure vessel with a stirring and heating system, add 100ml of pure water into the vessel, turn on the stirring and heating steam, and heat to 140°C. Control the pressure to 0.36Mpa and maintain it for 30min. Use nitrogen to press the solid-liquid mixture in the container into the pressure filter to filter, remove the activated carbon, cool the obtained clear liquid to 80°C and keep it for 2 hours, and then slowly cool down to 20°C. The cooling speed is controlled. Use a centrifuge to dehydrate the wet filter cake at 20°C / hour, rinse the wet filter cake with pure water for 1 minute, and after centrifuging again, put the filter cake in an oven to control the temperature at 100-105°C, and dry it for 2-4 hours to obtain 9.7g di Elemental acid boutique. The analysis results are shown in Table 1.

Embodiment 2

[0016] Example 2 : Add 20g of crude dodecanedibasic acid and 2g of activated carbon with an average particle size of 300 mesh into a pressure vessel with a stirring and heating system, add 100ml of pure water into the vessel, turn on stirring and heating steam, and heat to 170°C , control the pressure at 0.80Mpa and maintain it for 30min, press the solid-liquid mixture in the container into the pressure filter with nitrogen to filter, remove the activated carbon, cool the obtained clear liquid to 80°C and keep it for 2 hours, then slowly cool down to 20°C, the cooling speed Control the temperature at 20°C / hour, centrifuge and dehydrate with a centrifuge, rinse the wet filter cake with pure water for 2 minutes, and after centrifuging again, put the filter cake in an oven to control the temperature at 100-105°C, and dry it for 2-4 hours to obtain 19.5g Dibasic acid boutique. The analysis results are shown in Table 1.

Embodiment 3

[0017] Example 3: Add 30g of crude dodecanedibasic acid and 3g of activated carbon with an average particle size of 300 mesh into a pressure vessel with a stirring and heating system, add 100ml of pure water into the vessel, turn on the stirring and heating steam, and heat to 190°C. Control the pressure at 1.3Mpa and maintain it for 30 minutes, press the solid-liquid mixture in the container into the pressure filter with nitrogen to filter, remove the activated carbon, cool the obtained clear liquid to 80°C and keep it for 2 hours, then slowly cool down to 20°C, the cooling speed is controlled Use a centrifuge to dehydrate the wet filter cake at 20°C / hour, rinse the wet filter cake with pure water for 2 minutes, and after centrifuging again, put the filter cake in an oven to control the temperature at 100-105°C and dry it for 2-4 hours to obtain 29.0 g of Elemental acid boutique. The analysis results are shown in Table 1.

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Abstract

The invention discloses a C12-C13 long-chain binary acid refining method, which comprises the steps of: adding crude C12-C13 long-chain binary acid produced through a biological fermentation process into a dissolving tank and adding activated carbon or resin into the dissolving tank at the same time; adding purified water or deionized water into the dissolving tank, agitating and heating to enable the binary acid to be fully dissolved in the water and insoluble substances to be absorbed by the activated carbon or the resin; using nitrogen to press solid-liquid mixtures in the dissolving tank into a pressure-resistant filter and removing the activated carbon to obtain clear liquid; cooling the clear liquid and using a centrifuge for centrifugal dehydration to obtain a wet filter cake; and using purified water or deionized water to wash the wet filter cake and drying the filter cake to obtain the refined binary acid. By using a low-cost, nontoxic, hazard-free, safe and environment-friendly solvent to refine the crude long-chain binary acid, the refined long-chain binary acid which can be used for a subsequent polymerization process is obtained.

Description

technical field [0001] The present invention relates to the process of producing long-chain dibasic acid by microbial fermentation in the field of biochemical industry, in particular to C 12 -C 13 Process for refining long-chain dibasic acids. Background technique [0002] Long-chain dibasic acid is a fine chemical product with important and extensive industrial uses. Important raw materials for plasticizers, resins, medicines and pesticides. Long-chain dibasic acids with more than 10 carbons do not exist alone in nature, and there are three sources of them. 1. Production by pyrolysis of vegetable oil: some long-chain dibasic acids can be produced by pyrolysis of vegetable oil, but its purity is only about 70%, and its output is not large due to the constraints of farmland and climate conditions. 2. Preparation by chemical synthesis: All long-chain dibasic acids cannot be directly oxidized from n-alkanes in petroleum by chemical methods, because during chemical oxidation...

Claims

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Application Information

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IPC IPC(8): C07C55/02C07C51/42C07C55/21
Inventor 卢利玲洪军业桂秋芬王毅
Owner CHINA PETROLEUM & CHEM CORP
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