A kind of preparation method of 2,4-hexadienoic acid

A technology of hexadienoic acid and hexadienoic acid polyester, applied in 2 fields, can solve the problems of large amount of waste water, depolymerization yield of only 80%, and difficult treatment of salty waste water, etc., and achieves the effect of high yield of finished products

Active Publication Date: 2016-02-17
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] Embodiment 1: composite solid acid catalyst Pt-WO of the present invention 3 / ZrO 2 The preparation method:

[0044] 7.62gZrO(NO 3 ) 2 Make an aqueous solution, and then add ammonia water to obtain Zr(OH) 4 Precipitate, then filter, wash, dry, grind, impregnate with 104.75g ammonium tungstate for 6-8 hours, finally dry and roast to obtain WO 3 / ZrO 2 .

[0045] With cyclohexane as the continuous phase, cetyltrimethylammonium bromide (CTAB) as the surfactant, n-hexanol as the co-surfactant, 5.13ml, 0.15mol / L of 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 break the emulsification, separate, dry, and roast the solid at 400-550 degrees to obtain 100g of Pt-loaded WO 3 / ZrO 2 Solid super acid. The mass fraction of Pt is 0.15%, and the mass fraction of Z...

Embodiment 2

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

[0047] 6.35gZrO(NO 3 ) 2 Make an aqueous solution, and then add ammonia water to obtain Zr(OH) 4 Precipitate, then filter, wash, dry, and finely grind, then impregnate with 105.42g ammonium tungstate for 6-8 hours, and finally dry and roast to obtain WO 3 / ZrO 2 .

[0048] Using cyclohexane as the continuous phase, cetyltrimethylammonium bromide (CTAB) as the surfactant, n-hexanol as the co-surfactant, and 3.38ml, 1mol / L NiCl 2 Solution and 109.68g mass fraction are 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 break the emulsion, 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...

Embodiment 3

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

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

[0051] With cyclohexane as the continuous phase, nonylphenol polyoxyethylene ether (TX-10) as the surfactant, n-butanol as the co-surfactant, 3.38ml, 1mol / L NiCl 2 The solution and ammonia water form a microemulsion system as the water phase, and the prepared MoO is added to the microemulsion system 3 / MnO 2 , add tetrahydrofuran under stirring to break the emulsion, 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, which comprises the following steps in sequence: using glacial acetic acid as a raw material, obtaining vinyl ketone through high-temperature cracking at 700-800°C; condensing the obtained vinyl ketone with β-methacrolein to obtain 2 , 4-hexadienoic acid polyester; depolymerize the obtained 2,4-hexadienoic acid polyester under the catalysis of a composite solid acid catalyst to obtain crude 2,4-hexadienoic acid, and obtain the product 2,4-hexadienoic acid after post-processing. The method completely hydrolyzes 2,4-hexadienoic acid polyester, improves the depolymerization yield of 2,4-hexadienoic acid polyester, and the single depolymerization yield reaches 90%, and the finished product yield is high, and the unreacted β-methylpropene Aldehyde, solvent and ethanol solution can be recycled, no salty waste water is generated, and clean production is truly realized.

Description

technical field [0001] The invention belongs to the field of chemical production, and in particular relates to a preparation method of 2,4-hexadienoic acid. Background technique [0002] 2,4-Hexadienoic acid, the appearance is usually white needle-like or powdery crystals, 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 a kind of unsaturated fatty acid with conjugated diene, it can effectively inhibit the activity of mold, yeast and aerobic bacteria, and its effect of inhibiting the development and reproduction of harmful microorganisms is stronger than that of bactericidal, it is the food of the United Nations Preservatives recommended by the organization to countries around the world. 2,4-Hexadienoic acid has been widely used in antisepsis and preservation in various industries such as food, vegetables, fruits, ...

Claims

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Application Information

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Patent Type & Authority Patents(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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