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Method for preparing iso-octyl palmitate

A technology for isooctyl palmitate and palmitic acid, applied in the field of preparing isooctyl palmitate, can solve the problems of complex post-processing procedures, strong oxidizing property of concentrated sulfuric acid, strong acidity of concentrated sulfuric acid, etc., and achieves environmental friendliness and equipment investment. And the effect of low operating cost and high catalytic activity

Active Publication Date: 2010-06-23
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, most of the existing manufacturers of isooctyl palmitate in my country use concentrated sulfuric acid as a catalyst. Although concentrated sulfuric acid has ideal catalytic activity as an esterification catalyst, it has the following disadvantages: (1) concentrated sulfuric acid is strong in acidity, and during the production process The equipment is seriously corroded, which leads to frequent equipment replacement and increased production costs; (2) concentrated sulfuric acid has strong oxidative properties, resulting in alcohol dehydration to generate ether and coke, which affects product quality; (3) a large amount of waste acid and waste water pollution are generated during the production process environment; (4) concentrated sulfuric acid can not be recycled as a catalyst, which increases the production cost accordingly; (5) concentrated sulfuric acid is not easy to separate from the product, the post-treatment process is complicated, and the product cost increases

Method used

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  • Method for preparing iso-octyl palmitate
  • Method for preparing iso-octyl palmitate
  • Method for preparing iso-octyl palmitate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Esterification reaction: In a 100mL four-neck flask equipped with a stirrer, reflux condenser, and dropping funnel, add 0.078mol of palmitic acid and 5mL of isooctyl alcohol, and add 3 / 4 cyclohexane, nitrogen protection. Heat with an oil bath. After the palmitic acid is completely melted, add 0.525g of stannous oxalate solid acid catalyst and 5mL of cyclohexane, heat and reflux under normal pressure and stir. When the water produced by the reaction is separated from the water separator, start Timing, the reaction temperature is 150°C, and then 13.5mL of isooctyl alcohol is evenly and slowly added dropwise to the reactor through the dropping funnel, and the reaction stops when it enters the water separator until there is no water. The reaction time is 3.5 hours, and the isooctyl palmitate is obtained. The ester crude product is 30.5g, and the acid value is determined by sampling. The determination of the acid value adopts KOH solution as a standard solution and pheno...

Embodiment 2-5

[0030] Except following difference, all the other operations are identical with embodiment 1, and the addition of palmitic acid is identical with that in embodiment 1, and the amount of substance of palmitic acid and isooctyl alcohol is as shown in table 1:

[0031] Table 1

[0032] Example

Embodiment 6-9

[0034] Difference with embodiment 1 is that change catalyst consumption, preparation process is identical with the method for embodiment 1, and the percentage of catalyst consumption and palmitic acid and isooctyl alcohol feeding quality is as shown in table 2:

[0035] Table 2

[0036] Example

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PUM

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Abstract

The invention relates to a method for preparing iso-octyl palmitate shown in the formula (III), which comprises the following steps: in the nitrogen atmosphere, making palmitic acid shown in the formula (I) and isooctyl alcohol shown in the formula (II) react with a solid-acid catalyst for 2 to 6 hours at a temperature of between 100 and 180 DEG C; using a water segregator to add a water-carrying agent to carry out water carrying in the reaction process; and carrying out post-treatment on reaction solution after the reaction is finished to obtain the iso-octyl palmitate shown in the formula (III), wherein an amount-of-substance ratio of the total charging of the palmitic acid and the isooctyl alcohol is 1:1-4, the solid-acid catalyst is stannous oxalate, SO42- / ZrO2-Al2O3 or SO42- / TiO2-SnO2-Al2O3, and the usage of the solid-acid catalyst is 1 to 5 percent of the total charging mass of the palmitic acid and the isooctyl alcohol. The invention has the advantages of mild reaction condition, adoption of solid acid serving as the catalyst, reusable property, low equipment investment and operation cost and the like.

Description

(1) Technical field [0001] The invention relates to a method for preparing isooctyl palmitate, in particular to a method for preparing isooctyl palmitate by using a solid acid as a catalyst, and stannous oxalate is particularly recommended as a solid acid catalyst to prepare isooctyl palmitate. (2) Background technology [0002] Isooctyl palmitate, the solution is transparent and has no peculiar smell. It can be miscible with vegetable oil or mineral oil. It is not easy to oxidize, does not change color, and has good stability. Irritant, non-ionic surfactant that does not produce allergic reactions. [0003] The skin has a good absorption of isooctyl palmitate, and can closely contact with the hair follicles in the cortex, penetrate deep into the cortex, and bring the active ingredients into it, so as to fully exert the effect of the active ingredients. Adding isooctyl ester to cosmetics (the dosage is 2% to 5%) can make the product evenly spread on the skin, making the ski...

Claims

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Application Information

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IPC IPC(8): C07C69/24C07C67/08
Inventor 陈立军史鸿鑫周玲武宏科项菊萍
Owner ZHEJIANG UNIV OF TECH
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