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Preparation method of 2, 4-hexadienoic acid

A technology of hexadienoic acid and hexadienoic acid polyester, which is applied in two fields, can solve the problems of large amount of wastewater, difficult treatment of salty wastewater, and only 80% depolymerization yield, and achieve the effect of high yield of finished products

Active Publication Date: 2014-02-26
NANTONG ACETIC ACID CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Concentrated hydrochloric acid, concentrated sulfuric acid, etc. are the main depolymerization catalysts used in the existing process, and the depolymerization yield is only 80%, the waste water is large, and the salty waste water is difficult to treat.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Example 1: The composite solid acid catalyst Pt-WO of the present invention 3 / ZrO 2 Preparation method:

[0044] Add 7.62gZrO(NO 3 ) 2 Make it into an aqueous solution, then add ammonia to make Zr(OH) 4 Precipitate, then filter, wash, dry, grind, immerse in 104.75g ammonium tungstate for 6-8 hours, and finally dry and roast to prepare WO 3 / ZrO 2 .

[0045] Using cyclohexane as the continuous phase, cetyltrimethylammonium bromide (CTAB) as the surfactant, n-hexanol as the co-surfactant, with 5.13ml, 0.15mol / L chloroplatinic acid (H 2 PtCl 6 ) Solution and 104.21g of 40% hydrazine hydrate (N 2 H 4 ·H 2 O) The water phase constitutes a microemulsion system, and the prepared WO is added to the microemulsion system 3 / ZrO 2 , Add tetrahydrofuran under stirring to demulsify, separate, dry, and roast the solid at 400-550 degrees to obtain 100g of WO loaded with Pt 3 / ZrO 2 Solid super acid. The mass fraction of Pt is 0.15%, and the mass fraction of Zr is 3%.

Embodiment 2

[0046] Example 2: The composite solid acid catalyst Ni-WO of the present invention 3 / ZrO 2 Preparation method:

[0047] Add 6.35gZrO(NO 3 ) 2 Make it into an aqueous solution, then add ammonia to make Zr(OH) 4 Precipitate, then filter, wash, dry, grind, and then immerse in 105.42g ammonium tungstate for 6-8 hours, and finally dry and roast to prepare WO 3 / ZrO 2 .

[0048] Using cyclohexane as the continuous phase, cetyltrimethylammonium bromide (CTAB) as the surfactant, n-hexanol as the co-surfactant, with 3.38ml, 1mol / L NiCl 2 Solution and 109.68g of 40% hydrazine hydrate (N 2 H 4 ·H 2 O) The water phase constitutes a microemulsion system, and the prepared WO is added to the microemulsion system 3 / ZrO 2 , Add tetrahydrofuran under stirring to demulsify, separate, dry, and roast the solid at 400-550 degrees to obtain 100g of Ni-loaded WO 3 / ZrO 2 Solid super acid. The mass fraction of Ni is 0.2%, and the mass fraction of Zr is 2.5%.

Embodiment 3

[0049] Example 3: The composite solid acid catalyst Ni-MoO of the present invention 3 / MnO 2 Preparation method:

[0050] 6.87gMnCl 2 Make an aqueous solution, then add ammonia to make Mn(OH) 4 Precipitate, then filter, wash, dry, grind, and then immerse in 116.55g ammonium molybdate for 6-8 hours, and finally dry and roast to prepare MoO 3 / MnO 2 .

[0051] Using cyclohexane as the continuous phase, nonylphenol polyoxyethylene ether (TX-10) as the surfactant, n-butanol as the co-surfactant, with 3.38ml, 1mol / L NiCl 2 The solution and ammonia are the water phase to form a microemulsion system, and the prepared MoO is added to the microemulsion system 3 / MnO 2 , Add tetrahydrofuran under stirring to demulsify, separate, dry, and roast the solid at 400-550 degrees to prepare Ni-loaded MoO 3 / MnO 2 Solid super acid. The mass fraction of Ni is 0.2%, and the mass fraction of Mn is 3%.

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Abstract

The invention provides a preparation method of 2, 4-hexadienoic acid. The method sequentially comprises the following steps: with glacial acetic acid as a raw material, pyrolyzing the glacial acetic acid at the high temperature of 700-800 DEG C to obtain ketene; condensing the obtained ketene with beta-methylacrolein to obtain 2, 4-hexadienoic acid polyester; and depolymerizing the obtained 2, 4-hexadienoic acid polyester under the catalysis of a composite solid acid catalyst to obtain a 2, 4-hexadienoic acid crude product, thus obtaining a 2, 4-hexadienoic acid product through aftertreatment. The method has the advantages that the 2, 4-hexadienoic acid polyester is completely hydrolyzed, so that the depolymerization yield of the 2, 4-hexadienoic acid polyester is increased, the single depolymerization yield is up to 90% and the finished product yield is high; the unreacted beta-methylacrolein, a solvent and an ethanol solution can be recycled and no salt-containing wastewater is produced, so that clean production is truly realized.

Description

Technical field [0001] The invention belongs to the field of chemical production, and specifically relates to a preparation method of 2,4-hexadienoic acid. Background technique [0002] 2,4-hexadienoic acid, usually white needle-like or powder-like crystals in appearance, slightly soluble in water, soluble in many organic solvents. Molecular weight: 112.13; melting point: 132-135°C; boiling point: 228°C (decomposition); density: 1.204 (19°C); flash point: 127°C. This product is an unsaturated fatty acid with conjugated diene. It can effectively inhibit the activity of molds, yeasts and aerobic bacteria. Its inhibitory effect on the development and reproduction of harmful microorganisms is stronger than that of sterilization. It is the food of the United Nations. The preservative recommended by the organization to countries around the world. 2,4-hexadienoic acid has been widely used in various food, vegetables, fruits, medicine, rubber, papermaking, animal feed, cosmetics, paint...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C27/02C07C57/10B01J23/652B01J23/888B01J23/889B01J23/755B01J23/75
CPCB01J23/6525B01J23/6527B01J23/75B01J23/755B01J23/888B01J23/8898C07C51/09C07C57/10
Inventor 丁彩峰朱小刚刘芳姚俊生
Owner NANTONG ACETIC ACID CHEM
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