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Preparation method of isopropyl citrate

A technology of isopropyl citrate and citric acid, which is applied in the field of preparation of isopropyl citrate, can solve problems such as equipment corrosion, strong acidity of concentrated sulfuric acid, hidden safety hazards, etc., achieve mild esterification reaction conditions, improve reaction efficiency, Ease of recycling

Active Publication Date: 2021-05-28
蚌埠丰原涂山制药有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, isopropyl citrate is usually formed by esterification of citric acid and isopropanol under the catalysis of a catalyst. The current traditional production process uses concentrated sulfuric acid as a catalyst, but concentrated sulfuric acid is strong in acidity, and the production process is harmful to equipment. Corrosion is serious, there are certain safety hazards, and there are many side reactions when using concentrated sulfuric acid as a catalyst, the post-treatment process is complicated and the waste acid pollutes the environment
[0004] CN101270045A discloses a kind of method that takes hydrophobic solid acid as catalyst to synthesize citrate triester, it adopts hydrophobic solid acid as catalyst, prepares the citric acid triester of the alcohol of 1-3 C atom, adds in reaction process water agent, and adopt the method of batch sampling, although the post-treatment process is simplified to a certain extent, but the introduction of water-carrying agent increases the reaction cost to a certain extent

Method used

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  • Preparation method of isopropyl citrate

Examples

Experimental program
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Effect test

Embodiment 1

[0050] This example provides a method for preparing immobilized p-benzenesulfonic acid.

[0051] Take 20g of sodium alginate, 50g of polyvinyl alcohol, and 5g of p-toluenesulfonic acid and add them to 400mL of purified water, mix them evenly, and heat them in a constant temperature water bath at 90°C to dissolve them completely. After cooling to about 35°C, add 400mL of Add 2% calcium chloride solution dropwise to the above solution and keep stirring slowly. After the dropwise addition, place the reaction solution at 4°C for cross-linking for 24 hours, take it out, filter, dry under reduced pressure at 45°C for 5 hours, and pass through 60 mesh Sieve out fine particles to obtain immobilized p-toluenesulfonic acid.

Embodiment 2-3

[0053] This example provides a method for preparing immobilized p-benzenesulfonic acid.

[0054] The difference with Example 1 is that in this example, the mass ratio of sodium alginate, polyvinyl alcohol and p-benzenesulfonic acid is 1:10:1 (Example 2), 7:10:1 (Example 3) .

Embodiment 4

[0056] This example provides a method for activating a strong acid cation exchange resin.

[0057] Add 100g of strong acid cation exchange resin to 200mL of 5% sodium hydroxide and soak for 30min, wash with water until neutral, add 300mL of 5% hydrochloric acid to activate and soak for 30min, add purified water to wash until the effluent is neutral, filter, and vacuum dry at 50°C. Instantly.

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Abstract

The invention provides a preparation method of isopropyl citrate, wherein the preparation method comprises the following step: performing esterification reaction on citric acid and isopropanol under the catalysis of a solid acid catalyst to obtain the isopropyl citrate, wherein the solid acid catalyst is selected from immobilized p-benzenesulfonic acid and / or strong acid type cation exchange resin. The preparation method of isopropyl citrate provided by the invention is simple and easy to implement, post-treatment is convenient, and only simple filtration is needed to distill out low-boiling-point substances; the preparation method provided by the invention can improve the reaction efficiency of esterification reaction, and has no corrosion to equipment, the catalyst is easy to recycle, and the activity is basically kept unchanged.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and relates to a preparation method of isopropyl citrate. Background technique [0002] Isopropyl citrate is a mixture of monoisopropyl citrate, diisopropyl citrate and triisopropyl citrate, among which monoisopropyl citrate has the highest proportion, accounting for about 70%. Propyl esters interact with trace metals in fats to form inactive compounds that prevent oxidation. At present, isopropyl citrate is mainly used as an antioxidant and chelating agent, and can be used in oils and butter to prevent rancidity. [0003] At present, isopropyl citrate is usually formed by esterification of citric acid and isopropanol under the catalysis of a catalyst. The current traditional production process uses concentrated sulfuric acid as a catalyst, but concentrated sulfuric acid is strong in acidity, and the production process is harmful to equipment. The corrosion is serious, and there are c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/704C07C67/08B01J31/06B01J31/08
CPCC07C67/08B01J31/06B01J31/08C07C69/704Y02P20/584
Inventor 杜明松
Owner 蚌埠丰原涂山制药有限公司
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