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Method for preparing high-grade sucrose fatty acid ester from woody oil

A technology of sucrose fatty acid esters and fatty acid esters, which is applied in the field of preparing high-grade sucrose fatty acid esters, can solve the problems of restricting the industrial production and market application of sucrose fatty acid esters, restricting the market application of sucrose fatty acid esters, and the composition of sucrose fatty acid esters Complexity and other issues, to achieve the effect of low raw material cost, simple and feasible operation, and strong process operability

Inactive Publication Date: 2013-02-27
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Limit the industrial production and market application of sucrose fatty acid ester
[0006] 2. If oil is directly used as raw material or fatty acid methyl ester obtained by transesterifying woody oil with methanol or ethanol as raw material, the prepared sucrose fatty acid ester has complex components, often including sucrose stearate, sucrose Many types of sucrose fatty acid esters such as palmitate and sucrose linoleate and their mixtures of monoesters, diesters, triesters and polyesters are extremely unstable in performance, which limits the market application of sucrose fatty acid esters
[0007] 3. Many complex refining processes are required, the process is lengthy, the catalyst and solvent cannot be recovered, the industrial cost is high, the environmental pollution is serious, and the industrial feasibility is not high

Method used

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  • Method for preparing high-grade sucrose fatty acid ester from woody oil
  • Method for preparing high-grade sucrose fatty acid ester from woody oil
  • Method for preparing high-grade sucrose fatty acid ester from woody oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The first step is the hydrolysis of woody oil, the molar ratio of soybean oil to sodium hydroxide is 1: 3, methanol is slightly excessive, NaOH is dissolved in distilled water and added to the three-necked flask together with methanol, and the oil is added dropwise from the separatory funnel at a constant speed Transfer to a three-necked flask, mechanically stir evenly, add dropwise at 60°C for 3 hours, keep warm for 2 hours, cool to room temperature, add hydrochloric acid dropwise to a pH value of 3 to 4, leave to stand at room temperature and separate layers, the lower layer is the crude glycerin phase, recover and extract the glycerin, The upper layer is crude fatty acid, to be separated.

[0041] The second step is the separation of free fatty acids. Mix and seal the separated upper crude fatty acids with methanol at a mass ratio of 1:3, pre-cool at 0°C and freeze at -20°C for 2 hours each, filter at low temperature to obtain a clear filtrate, and dissolve the filter...

Embodiment 2

[0044] The first step, the hydrolysis of woody oil, the molar ratio of soybean oil to sodium hydroxide is 1: 2, low-carbon alcohol is slightly excessive, NaOH is dissolved in distilled water and added to a three-necked flask together with ethanol, and the oil is discharged from the separatory funnel at a constant rate. Add dropwise to a three-necked flask, mechanically stir evenly, add dropwise at 70°C for 1.5h, keep warm for 1.5h, cool to room temperature, add hydrochloric acid dropwise to pH 3-4, stand at room temperature and separate layers, the lower layer is the crude glycerin phase, Glycerin can be recovered and extracted, and the upper layer is crude fatty acid to be separated.

[0045] The second step is the separation of free fatty acids. Mix and seal the separated upper crude fatty acids and ethanol at a mass ratio of 1:4, pre-cool at 0.5°C and freeze at -17.5°C for 2 hours each, filter at low temperature to obtain a clear filtrate, and dissolve the filter cake After...

Embodiment 3

[0048] The first step, the hydrolysis of woody oil, the mol ratio of soybean oil and sodium hydroxide is 1: 1, slightly excess ethanol, after dissolving NaOH in distilled water, add three-necked flask together with n-propanol, grease is from separating funnel constant speed Add dropwise to a three-necked flask, mechanically stir evenly, dropwise react at 80°C for 0.5h, keep warm for 1h, cool to room temperature, add hydrochloric acid dropwise to pH 3-4, stand at room temperature and separate layers, the lower layer is the crude glycerin phase, Glycerin can be recovered and extracted, and the upper layer is crude fatty acid to be separated.

[0049] The second step is the separation of free fatty acids. Mix and seal the separated upper crude fatty acids and n-propanol at a mass ratio of 1:5, pre-cool at 1°C and freeze at -15°C for 2 hours each, and filter at low temperature to obtain a clear filtrate. After the cake is dissolved, it is distilled under reduced pressure to obtain...

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Abstract

The invention provides a method for preparing high-grade sucrose fatty acid ester from woody oil, comprising the following steps of: mixing woody oil, lower alcohol and an aqueous sodium hydroxide solution for reacting, after the reaction is ended, regulating the pH value to be faintly acid, standing for demixing, separating out a liquid at the upper layer and a hydrous crude glycerol phase at the lower layer; then mixing the liquid at the upper layer with the lower alcohol for sealing, freezing at low temperature, then filtering to obtain a clear filtrate, dissolving filter cakes, and then carrying out reduced pressure distillation to obtain a saturated fatty acid; mixing the clear filtrate with urea, heating until the mixture is dissolved, filtering after freezing at low temperature, rotatably evaporating the filtrate, then dissolving with a non-polar solvent, filtering, rotatably evaporating the filtrate to obtain polyunsaturated fatty acids; and finally, under the protection of N2, mixing the separated fat acids with sucrose, a cosolvent and a catalyst, heating for reacting, and refining the reaction mixture with a two-phase extraction method to obtain the sucrose fatty acid ester. The invention has the characteristics of easy obtaining of rich raw materials, low cost, easy separation of product, stable performance, high purify, and the like.

Description

technical field [0001] The invention belongs to the technology of synthesizing sucrose fatty acid ester, in particular to a method for preparing high-grade sucrose fatty acid ester from woody oil. Background technique [0002] As a new type of natural non-ionic surfactant, sucrose fatty acid ester is non-toxic and harmless to human body and nature, can be degraded and absorbed by human body and nature, and has good emulsification, dispersion, solubilization, penetration, foaming, viscosity Adjustment, anti-aging, antibacterial and other properties, are widely used in food, medicine, chemical industry, cosmetics, detergents, textiles and agriculture and animal husbandry and other industries. It has been successively approved by Japan, the United States, China and other countries as well as the Food and Agriculture Organization of the United Nations, the World Health Organization, and the European Union as food additives and co-solvents. It has huge market demand and broad app...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H13/06C07H1/00
Inventor 蒋剑春王奎吕薇徐俊明应浩
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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