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Solid acid catalyst for transesterification, preparation method of solid acid catalyst and preparation method of vitamin A palmitate

A solid acid catalyst, a technology for transesterification, which is used in the preparation of the mutual reaction between ester groups, chemical instruments and methods, catalysts for physical/chemical processes, etc. Achieve the effect of solving mechanical performance problems, avoiding a large amount of loss, and simple process

Active Publication Date: 2021-03-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

BASF patent GB1293041 discloses a kind of acid chloride method, after palmitic acid is acylated by thionyl chloride, reacts with VA alcohol in the presence of acid-binding agent (triethyl gum, pyridine, etc.) Fast, high product yield, etc., but the reaction has disadvantages such as high energy consumption, severe corrosion of equipment due to the generation of HCl gas after the reaction, high toxicity of palmitoyl chloride, serious pollution, and difficult separation of acid-binding agents.
In addition, the product is easily destroyed under the influence of acidic medium to form dehydrated VA crystals, which affects product performance

Method used

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  • Solid acid catalyst for transesterification, preparation method of solid acid catalyst and preparation method of vitamin A palmitate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Modified Catalyst S 2 o 8 2- / Fe 3+ -CNT@Ni 3 Preparation of PO:

[0050] (1) Dissolve 1 mol of nickel acetylacetonate in a mixed solution of 500 mL of deionized water and ethylene glycol (the volume ratio of water to ethylene glycol is 0.4:1), and stir thoroughly. Add a 1% potassium carbonate aqueous solution dropwise, add dropwise for 1 hour to adjust the pH of the solution to 7.5, add 4 mol of triphenylphosphine to the above solution, reflux at 300°C for 4 hours, and dry the obtained precipitate under nitrogen blanketing for use.

[0051] (2) 20g of carbon nanotube powder is placed in 100ml of 98% concentrated sulfuric acid, immersed at 100°C for 5h, filtered, and the filtered black solid is placed in 500mL, 1mol / L ferric chloride aqueous solution to obtain a yellow slurry , and the obtained solid was filtered and dried under the protection of nitrogen for further use. The metal content in the obtained metal-doped modified carbon nanotubes was measured by ICP t...

Embodiment 2

[0055] Modified Catalyst S 2 o 8 2- / Fe 3+ -CNT@Ni 3 Preparation of PO:

[0056] (1) Dissolve 1 mol of nickel acetylacetonate in a mixed solution of 500 mL of deionized water and ethylene glycol (the volume ratio of water to ethylene glycol is 0.5:1), and stir thoroughly. Add a 2% potassium carbonate aqueous solution dropwise, add dropwise for 1 hour to adjust the pH of the solution to 8.0, add 5 mol of triphenylphosphine to the above solution, reflux at 400° C. for 5 hours, and dry the obtained precipitate under nitrogen blanketing for use.

[0057] (2) 30g of carbon nanotube powder is placed in 100ml of 98% concentrated sulfuric acid, soaked at 110°C for 6h, filtered, and the resulting black solid is placed in 500mL, 1.3mol / L ferric chloride aqueous solution to obtain a yellow slurry, The resulting solid was filtered and dried under nitrogen protection for future use. The metal content in the obtained metal-doped modified carbon nanotubes was measured by ICP to be 7.5 ...

Embodiment 3

[0061] Modified Catalyst S 2 o 8 2- / Fe 3+ -CNT@Co 3 PO 2 Preparation of:

[0062] (1) Dissolve 1 mol of cobalt acetylacetonate in a mixed solution of 500 mL of deionized water and ethylene glycol (the volume ratio of water to ethylene glycol is 0.6:1), and stir thoroughly. Add a 3% potassium carbonate aqueous solution dropwise, add dropwise for 1 hour to adjust the pH of the solution to 8.2, add 6 mol of triphenylphosphine to the above solution, reflux at 500° C. for 6 hours, and dry the resulting precipitate under nitrogen for use.

[0063] (2) 40g of carbon nanotube powder is placed in 100ml of 98% concentrated sulfuric acid, soaked at 120°C for 7h, filtered and taken out, and the resulting black solid is placed in 500mL, 1.7mol / L ferric chloride aqueous solution to obtain a yellow slurry , and the obtained solid was filtered and dried under the protection of nitrogen for further use. The metal content in the obtained metal-doped modified carbon nanotubes was measure...

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Abstract

The invention discloses a solid acid catalyst for transesterification, a preparation method of the solid acid catalyst and a preparation method of vitamin A palmitate. The catalyst is structurally marked as S2O8<2-> / MxPyOz@N<w+>-CNT, wherein S2O8<2-> is an active component, and MxPyOz is an oxygen-containing metal phosphide. According to the catalyst, the problem of mechanical properties of a solid acid catalyst is solved by utilizing blending modification of carbon nanotubes, active components are loaded on an amorphous oxygen-containing metal phosphorus compound, so that massive loss of theactive components of the traditional solid acid catalyst in a reaction system is avoided, and the acid strength of the catalyst is controlled by adopting a silane passivation technology, the serious problem that byproducts are generated in the transesterification process of a traditional solid acid catalyst is solved. The catalyst is used for preparation of vitamin A palmitate, and the process hasthe advantages of simple operation, high catalytic efficiency, environmental protection, and continuous production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a super strong solid acid catalyst for transesterification, a preparation method thereof, and a preparation method of vitamin A palmitate. Background technique [0002] Vitamin A palmitate (VA palmitate) is one of the main series of vitamin A products. Compared with vitamin A acetate (VA acetate), VA palmitate has a long carbon chain, low melting point and good oil solubility. It has good low temperature stability and is not prone to crystal precipitation. It is an indispensable substance for the normal metabolism of humans and animals. Due to its better stability and better pharmacological effects, it has been widely used in cosmetics, medicines, feeds, etc. [0003] VA palmitate is mainly prepared by biological enzyme method and chemical synthesis method. The bio-enzyme method mainly uses VA acetate as a raw material, and undergoes esterification or tran...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/02B01J27/185B01J23/745B01J21/18B01J35/10C07C67/02C07C69/24
CPCB01J27/02B01J27/1853B01J23/745B01J21/185C07C67/02C07C2601/16B01J35/615B01J35/647C07C69/24
Inventor 罗朝辉林龙翟文超吕英东黎源
Owner WANHUA CHEM GRP CO LTD
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