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Palmitoleic acid monoisopropanolamide synthesis method

A technology of monoisopropanolamide and palmitoleic acid is applied in the preparation of carboxylic acid amides, chemical instruments and methods, preparation of organic compounds, etc. Comparable, oleochemical field development constraints and other issues, to achieve the effects of low unit cost, low cost and simple preparation

Active Publication Date: 2015-12-09
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] Example 1: Preparation of solid silica supported metal oxide catalyst

[0015] First add 27.5g of potassium nitrate (approximately 0.272mol), 12.6g of zinc nitrate (approximately 0.06mol), and 8.6g (approximately 0.05mol) of magnesium nitrate into 250ml of deionized water. The solution is heated in a 70℃ water bath and stirred Dissolve. Take 100g of the silica carrier of 3~5mm and immerse it in the above-mentioned solution at 60°C in a water bath 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. Finally, place the dried catalyst on a tray and move it to a muffle furnace at 400°C for heating for 3 hours. After cooling, the reaction can be obtained. Metal oxide catalyst.

Embodiment 2

[0016] Example 2: Synthesis of palmitoleic acid monoisopropanolamide

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

[0018] The weight of the obtained product is 592.5, the yield is about 95.2%, and the average content of palmitoleic acid monoisopropanolamine is about 95%; other indicators of the product are as follows: pH is 8.6, total amine value is 18.0mgKOH / g, acid value It is 42.7mgKOH / g, and the conductivity (10% aqueous solution, us / cm...

Embodiment 3

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

[0020] Table 1 The influence of different synthesis processes on the total amine value of palmitoleic acid monoisopropanolamine

[0021] .

[0022] This application prepares a new type of solid silica supported metal oxide catalyst, which has low cost and simple 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 processed.

[0023] In the above solution provided by this application, the solid silica negative metal carrier is used as the catalyst, the catalyst unit cost is low, the reaction process conditions 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 ...

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PUM

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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 method for synthesizing palmitoleic acid monoisopropanolamide, and belongs to the technical field of organic synthesis. Background technique [0002] Palm oil is currently the world's largest oil, but because its synthetic chemicals are not as water-soluble as lauric acid products, and their oil solubility is not comparable to stearic acid products, the development in the oleochemical field is restricted. In view of the shortcomings of the aforementioned palm oil products, the hydrophilic and lipophilic properties of the products can be balanced by preparing palmitoleic acid amide compounds. Among them, palmitic acid monoisopropanolamide can be used as thickener, emulsifier, antistatic agent, fat-enriching agent, rust inhibitor, etc., and can also be used as an intermediate for the synthesis of many new and excellent surfactants. It is a widely used non-ionic surfactant with good washing properties such as thickening and foam sta...

Claims

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Application Information

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Patent Type & Authority Applications(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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