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Molecular distillation purification method of polyprenol

A technology of molecular distillation and polyprenol, which is applied in the direction of distillation purification/separation, chemical instruments and methods, organic chemistry, etc., can solve the problems of large residual amount of additives, large amount of solvent, and difficulty in distilling out, etc., to increase molecular weight Distillation speed, increased purity, and well-sourced effects

Inactive Publication Date: 2006-01-04
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

However, non-polar solvents (petroleum ether, ether, ethyl acetate, etc.) are used to detach the NKA resin, and the non-polar solvent dissolves the additives in the pores of the NKA resin. The residual amount of additives in the product is extremely large, and it is not easy to steam out
[0005] Therefore, there are three obvious disadvantages in the traditional method for separating and preparing polyprenol: 1. When silica gel and alumina are separated and prepared, the recycling of silica gel and alumina is a problem, and the cost is high
2. When different proportions of petroleum ether, ether, acetone, ethyl acetate and other mixed solvents are used for extraction and detachment column chromatography, not only the amount of solvent used is large, but also the loss and cost are high when recovering and separating the solvent
3. There is the residual problem of solvent in the prepared polyprenol product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Embodiment 1 A kind of molecular distillation purification method of polyprenol comprises the following two steps: the first step, grade I molecular distillation: the polyprenol content is lower than the ointment of 50% (Chinese Academy of Forestry Forestry Institute Science and Technology Developed by the head office) at a flow rate of 3ml / min~15ml / min, the vacuum degree is kept at 1×10 -2 mbar~10×10 -2 mbar, temperature is distilled in the molecular distillation evaporator (KDL5 type, German U.I.C.GMBH company production) of 80 ℃~160 ℃, in the present embodiment, flow velocity can be 5ml / min, 8ml / min, 10ml / min, 13.2ml / min, the vacuum can be 3×10 -2 mbar, 5×10 -2 mbar, 8×10 -2 mbar, the temperature can be 92°C, 105°C, 109°C, 117°C, 130°C, 142°C, 155°C, light oil-1 is distilled off, and the residue of class I molecular distillation can be obtained. The second step is class II molecular distillation : Send the first grade molecular distillation residue into the vacu...

Embodiment 2

[0019]Example 2 A molecular distillation purification method of polyprenol, including the following two steps: the first step, I-level molecular distillation: the ointment with a polyprenol content of less than 50% is developed by the Institute of Forestry, Chinese Academy of Forestry Produced by the head office) at a flow rate of 3ml / min~15ml / min, the vacuum degree is kept at 1×10 -2 mbar~10×10 -2 mbar, temperature is distilled in the molecular distillation evaporator (KDL5 type, German U.I.C.GMBH company production) of 80 ℃~160 ℃, in the present embodiment, flow velocity can be 5ml / min, 8ml / min, 10ml / min, 13.2ml / min, the vacuum can be 3×10 -2 mbar, 5×10 -2 mbar, 8×10 -2 mbar, the temperature can be 92°C, 105°C, 109°C, 117°C, 130°C, 142°C, 155°C, light oil-1 is distilled off, and the residue of class I molecular distillation can be obtained. The second step is class II molecular distillation : Send the first grade molecular distillation residue into the vacuum at a flow ...

Embodiment 3

[0020] Embodiment 3 A kind of molecular distillation purification method of polyprenol comprises the following two steps: the first step, grade I molecular distillation: the polyprenol content is lower than 50% ointment with 3ml / min~15ml / min The flow rate is fed into the vacuum and maintained at 1×10 -2 mbar~10×10 -2 mbar, temperature is distilled in the molecular distillation evaporator (KDL5 type, German U.I.C.GMBH company production) of 80 ℃~160 ℃, in the present embodiment, flow velocity can be 5ml / min, 8ml / min, 10ml / min, 13.2ml / min, the vacuum can be 3×10 -2 mbar, 5×10 -2 mbar, 8×10 -2 mbar, the temperature can be 92°C, 105°C, 109°C, 117°C, 130°C, 142°C, 155°C, light oil-1 is distilled off, and the residue of class I molecular distillation can be obtained. The second step is class II molecular distillation : Send the first grade molecular distillation residue into the vacuum at a flow rate of 5ml / min~15ml / min and keep it at 1×10 -3 mbar~5×10 -3 mbar, the temperatur...

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PUM

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Abstract

A process for purifying the polypentenol by molecular distillation includes such steps as feeding the raw polypentanol into a high-temp vacuum molecular distilling evaporator at a certani speed, distilling, feeding the distilled substance into another high-temp vacuum molecular distilling evaporator at a certain speed, and distilling to obtain the high-purity (70-95 mass%) product.

Description

technical field [0001] The invention relates to a plant polyprenol extraction and separation technology, in particular to a molecular distillation purification method of polyprenol. Background technique [0002] Polyprenol widely exists in higher plants. Our research shows that polyprenol mainly exists in ginkgo leaves and green needles such as Pinus massoniana, black pine, slash pine, juniper and cedar in China. The content in leaves is as high as 2.0%, followed by about 1.0% in needles such as masson pine, cedar, and black pine. Polyprenols are lipid compounds composed of a series of prenyl units and terminal prenol units. They all have the chemical structure of birch polyprenols (Butalpolyprenols), that is, ω-(trans)2-(cis)n-α (wherein n is 10-21, α is isopentenol), they are compatible with human body and breastfeeding The structure of dolichols contained in animal organs (Dolichols structure is ω-(trans)2-(cis)n-α, where n is 12-19, α is isoa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/02C07C29/80C07C7/04C07C35/06
Inventor 王成章沈兆邦刘妤婵
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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