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A kind of two-step method prepares the method for low free glycerol mono- and glyceryl distearate

A kind of glyceryl distearate, low free technology, applied in the direction of fatty acid esterification, carboxylate preparation, chemical instruments and methods, etc. The effect of improving product quality and decreasing free glycerin content

Active Publication Date: 2018-12-14
杭州赞宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The above-mentioned several processes all have shortcomings to varying degrees. At present, molecular distillation of high-purity glyceryl monostearate is basically used instead of glycerin mono- and distearate with low free glycerol. This not only increases the cost of use, but also affects the effect of use. influences

Method used

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  • A kind of two-step method prepares the method for low free glycerol mono- and glyceryl distearate
  • A kind of two-step method prepares the method for low free glycerol mono- and glyceryl distearate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 160g of glycerin and 0.8g of sodium hydroxide into the reactor equipped with heating, stirring, vacuum, and gas inlet and outlet devices, turn on the stirring, vacuum, and heating, and raise the temperature to 100°C with a vacuum of 0.09MPa to completely dissolve the sodium hydroxide in in glycerin.

[0033] Turn off the vacuum, add 650g of hydrogenated oil to react, pass in nitrogen and keep the nitrogen pressure at 0.08MPa; continue to heat up to 240°C, and react for 30 minutes; turn off the heating and start to cool down, while cooling down, slowly add 170g of hydrogenated oil at a uniform speed, and control the cooling rate to 3°C / min, at the end of the cooling, exactly 170g of hydrogenated oil has been added. After cooling down to 160°C, keep warm for 60 minutes, the reaction is over, and the product is obtained by cooling.

[0034] Example 1 Inspection data

[0035] project

Embodiment 2

[0037] Add 160g of glycerin and 1g of sodium hydroxide into the reactor equipped with heating, stirring, vacuum, and gas in and out devices, turn on stirring, vacuum, and heating, and raise the temperature to 100°C with a vacuum of 0.09MPa to completely dissolve the sodium hydroxide in the glycerin middle.

[0038] Turn off the vacuum, add 660g of hydrogenated oil to react, feed nitrogen and keep the nitrogen pressure at 0.08MPa; continue heating to 235°C, and react for 40min; turn off the heating and start to cool down, while cooling down, slowly add 170g of hydrogenated oil at a uniform speed, and control the cooling rate to 3°C / min, at the end of the cooling, exactly 170g of hydrogenated oil has been added. After cooling down to 150°C, keep it warm for 60 minutes, the reaction is over, and the product is obtained by cooling.

[0039] Embodiment 2 inspection data

[0040] project

Embodiment 3

[0042] Add 170g of glycerin and 0.8g of sodium hydroxide into the reactor equipped with heating, stirring, vacuum, and gas inlet and outlet devices, turn on the stirring, vacuum, and heating, and raise the temperature to 100°C with a vacuum of 0.09MPa to completely dissolve the sodium hydroxide in in glycerin.

[0043] Turn off the vacuum, add 650g of hydrogenated oil for reaction, feed nitrogen and keep the pressure of nitrogen at 0.08MPa; continue to heat up to 230°C, and react for 60 minutes; turn off the heating and start to cool down, while cooling down, slowly add 180g of hydrogenated oil at a uniform speed, and control the cooling rate to 3°C / min, at the end of cooling, exactly 180g of hydrogenated oil has been added. After cooling down to 160°C, keep warm for 50 minutes, the reaction is over, and the product is obtained by cooling.

[0044] Embodiment 3 inspection data

[0045]

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Abstract

The invention relates to a two-step method of producing glyceryl monostearate and glyceryl distearate with low free glycerol. The glyceryl monostearate and glyceryl distearate prepared through the method has high quality, high yield and low cost. The method includes the steps of: (1) adding glycerol and a catalyst into a reactor and stirring, vacuumizing and heating the components, and vacuum-heating the components until the catalyst is all dissolved in glycerol; (2) stopping vacuum equipment and adding hydrogenated oil to perform a reaction, feeding nitrogen gas and maintaining the pressure of the nitrogen gas, and continuously heating the components to perform a reaction; and (3) stopping heating to start temperature reduction, and at the same time, slowly adding the rest of the hydrogenated oil with temperature reduction speed and hydrogenated oil addition speed controlled, maintaining the temperature until the reaction is finished, and then cooling the reaction product to obtain the finish products.

Description

technical field [0001] The invention relates to the field of fine chemicals, in particular to a two-step method for preparing low-free glycerin mono- and distearic acid glycerides. Background technique [0002] Glyceryl monostearate and glyceryl distearate are a mixture of glyceryl monostearate, glyceryl distearate and a small amount of oil. It is a white waxy solid, insoluble in water, soluble in oil, paraffin, ethanol, chloroform, acetone , ether and other solvents, is a polyol-type non-ionic surfactant; it has both hydrophilic and lipophilic groups, and the hydrophilic-lipophilic balance value (referred to as HLB value) is 3.6 to 4.2. , daily chemical, textile, and pharmaceutical industries are the most widely used and used additives; it can be used as an emulsifier for food, cosmetics, and pharmaceutical ointments, a lubricant for plastics, and an antistatic agent. It can also be used as a defoamer, dispersant Agents, thickeners, wetting agents, etc. [0003] At presen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/003C07C69/30C07C67/03C07C67/08C11C3/06
CPCC07C67/03C07C67/08C11C3/06C07C69/003C07C69/30
Inventor 周建东计晓黎蒋海刚王晓辉
Owner 杭州赞宇化工有限公司
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