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A kind of synthetic method of palmitoleic acid monoisopropanolamide

A technology of monoisopropanolamide and palmitoleic acid, which is applied to the preparation of carboxylic acid amide, chemical instruments and methods, and the preparation of organic compounds. Comparable with stearic acid products and other issues, it achieves the effect of low unit consumption cost, low cost and simple preparation

Active Publication Date: 2017-04-12
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Palm oil is currently the world's largest oil and fat, but because the water solubility of synthetic chemicals is not as good as that of lauric acid products, and the oil solubility is not comparable to that of stearic acid products, the development in the field of oleochemicals is restricted.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Embodiment 1: Preparation of solid silica supported metal oxide catalyst

[0015] First, add 27.5g (about 0.272mol) of potassium nitrate, 12.6g (about 0.06mol) of zinc nitrate, and 8.6g (about 0.05mol) of magnesium nitrate into 250ml of deionized water, heat the solution in a water bath at 70°C, and stir dissolve. Take 100g of 3~5mm silica carrier and immerse in the above solution in a water bath at 60°C for 1 hour, and then remove the solvent under reduced pressure. Then place the dehydrated catalyst in a vacuum oven at 120°C for heating and drying, and finally put the dried catalyst on a tray and move it to a muffle furnace at 400°C for heating for 3 hours. metal oxide catalysts.

Embodiment 2

[0016] Embodiment 2: the synthesis of palmitoleic acid monoisopropanolamide

[0017] In a 2.0L glass-lined reactor, add 509g of palmitoleic acid (about 2mol), 165g of monoisopropanolamine (about 2.2mol), and 7.0g of silica-supported metal oxide catalyst, stir mechanically, and evacuate to -0.09MPa, heat up to 120°C to react for 3 hours, cool to about 80°C, vacuum again to -0.09MPa to recover the remaining monoisopropanolamine and water in the reaction kettle, and cool the waste liquid to the flask through the cooling tube , the time is about 45 minutes. The catalyst and the liquid are separated by filtration to obtain a yellow viscous liquid palmitoleic acid monoisopropanolamine.

[0018] Obtaining product weighing is 592.5 and yield is about 95.2%, and the average content of palmitoleic acid monoisopropanolamine is about 95%; Other indexes of product are as follows: pH is 8.6, and total amine value is 18.0mgKOH / g, acid value It is 42.7mgKOH / g, and the conductivity (10% aque...

Embodiment 3

[0019] Example 3: The synthetic process is adjusted, palmitoleic acid monoisopropanolamine prepared under different reaction conditions, see Table 1 for details.

[0020] Table 1 Effect of different synthesis processes on the total amine value of monoisopropanolamine palmitoleate

[0021] .

[0022] The present application prepares a novel catalyst with solid silicon dioxide supporting metal oxides. The catalyst is low in cost and simple in preparation. The reaction process conditions of palmitoleic acid monopropanolamide are mild, the product conversion rate is high, the catalyst after the reaction can be recycled and reused, and the product does not need to be post-treated.

[0023] In the above-mentioned scheme provided by the present application, the solid silica negative metal carrier is used as the catalyst, the unit cost of the catalyst is low, the reaction process conditions are mild, the product conversion rate is high, the catalyst after the reaction can be recycl...

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Abstract

The invention relates to a palmitoleic acid monoisopropanolamide synthesis method and belongs to the technical field of organic polymerization. The synthesis method comprises that palmitoleic acid and isopropanolamine as raw materials undergo a heating synthesis reaction in the presence of a solid metal oxide catalyst under condition of pressure reduction at a temperature of 100-150 DEG C for 1-5h, wherein a mole ratio of palmitoleic acid to isopropanolamine is 1: 1-1.5 and use mass of the catalyst is 2-10% the isopropanolamine mass. The synthesis method has the advantages of low catalyst unit consumption cost, mild reaction conditions, high product conversion rate, recovery and recycle of the reacted catalyst, and no use of an aftertreatment process.

Description

technical field [0001] The invention relates to a synthesis method of palmitoleic acid monoisopropanolamide, which belongs to the technical field of organic synthesis. Background technique [0002] Palm oil is currently the world's largest oil and fat, but because the water solubility of synthetic chemicals is not as good as that of lauric acid products, and the oil solubility is not comparable to that of stearic acid products, the development in the field of oleochemicals is restricted. In view of the shortcomings of the above-mentioned palm oil products, the hydrophilic and lipophilic properties of the product can be balanced by preparing palm oleic acid amide compounds. Among them, palmitic acid monoisopropanolamide can be used as a thickener, emulsifier, antistatic agent, fat-rich agent, antirust agent, etc., and can also be used as an intermediate for the synthesis of many new surfactants with excellent performance. It is a widely used non-ionic surfactant with good wa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/02C07C233/20B01J23/06
CPCY02P20/584
Inventor 宋明贵颜吉校金一丰郭玉峰俞芳
Owner ZHEJIANG HUANGMA TECH
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