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Preparation method used for preparing catalyst of polyglycerol and application thereof

A technology of polyglycerol and catalyst, applied in chemical instruments and methods, physical/chemical process catalysts, ether preparation, etc., can solve the problems of short reaction time, uneconomical, shortened reaction time, etc., achieve short reaction time and improve quality , the effect of expanding varieties

Inactive Publication Date: 2010-06-02
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] From an economic point of view, the preparation of polyglycerol with a large degree of polymerization is still the method of dehydration polymerization of glycerol under the action of a catalyst, and the catalysts used are mostly common alkaline substances, such as KOH, NaOH, K 2 CO 3 and Na 2 CO 3 Etc., as the degree of polymerization of the polyglycerin produced increases, the color of the product changes from yellow to dark brown, even black, and the smell becomes stronger and stronger, which cannot meet the quality requirements of the application.
[0008] In order to overcome the shortcomings of the above-mentioned catalysts, U.S. Patent No. 4,551,561 discloses a phosphate catalyst. Although the color of polyglycerol is obviously improved, the reaction speed is too slow to make the method uneconomical.
[0009] European Patent No. 732,318 discloses a metaaluminate catalyst, which can improve the color of polyglycerol and shorten the reaction time, but the polymerization activity is low, and only 2 to 3 polyglycerols can be prepared.
[0010] In view of the above-mentioned status quo, a catalyst for polyglycerol with high catalytic activity, short reaction time, and light color of polyglycerol with a degree of polymerization of 2 to 20 has not been found yet.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: γ-Al 2 o 3 -NaOH-Na / H 3 PO 3 Catalyst preparation

[0027] Add 20 grams of NaOH into a 250mL four-necked flask, make a 20wt% solution with 80 grams of deionized water, add 40 grams of γ-Al 2 o 3 , turn on the stirring device, heat up slowly, evaporate the water to dryness, transfer to an evaporating dish, put it in an oven at 120°C for drying for 12 hours, then transfer it to a crucible and bake at 500°C for 4 hours, and put it back into a four-neck flask , open the nitrogen channel, add 2 grams of sodium metal in batches at 350°C under the protection of nitrogen, continue the reaction for 1 hour, then cool to room temperature, and the alkalinity is greater than 35. Continue to add 10 grams of phosphorous acid under the protection of nitrogen and mix with a masher at 800-1000 rpm to obtain 68 grams of finished catalyst, which is bottled, filled with nitrogen and sealed for later use.

[0028] Preparation of polyglycerol:

[0029] Add 150 grams of glyce...

Embodiment 2

[0030] Example 2: γ-Al 2 o 3 -Na 2 CO 3 -Na / H 3 PO 2 Catalyst preparation

[0031] 16 g Na 2 CO 3 Add in a 250mL four-neck flask, make a 16wt% solution with 84 grams of deionized water, add 25 grams of γ-Al 2 o 3 , turn on the stirring device, heat up slowly, evaporate the water to dryness, transfer to a crucible, put it in an oven at 120°C for 12 hours, bake at 400°C for 8 hours, put it back into the four-necked flask, and open the nitrogen passage , under the protection of nitrogen, 4 grams of sodium metal was added in batches at 320° C., and the reaction was continued for 2 hours, then cooled to room temperature, and the alkalinity was determined to be 37. Add 9 grams of hypophosphorous acid under nitrogen protection and mix at a high speed with a masher at 800-1000 rpm to obtain 50 grams of finished catalyst, bottle it with nitrogen and seal it for use.

[0032] Preparation of polyglycerol:

[0033] Add 150 grams of glycerin in the 250mL four-neck flask with sti...

Embodiment 3

[0034] Example 3: γ-Al 2 o 3 -KOH-Na / H 3 PO 2 Catalyst preparation

[0035] Add 15 grams of KOH into a 250mL four-necked flask, make a 30wt% solution with 35 grams of deionized water, and add 15 grams of γ-Al 2 o 3 , turn on the stirring device, heat up slowly, evaporate the water to dryness, transfer to a crucible, put it in an oven at 120°C for 12 hours, bake it at 480°C for 5 hours, put it back into the four-necked flask, and open the nitrogen passage , under the protection of nitrogen, 3 grams of sodium metal was added in batches at 380 ° C, and the reaction was continued for 2 hours, then cooled to room temperature, and the alkalinity was measured to be about 37. Add 6 grams of hypophosphorous acid under nitrogen protection and mix at high speed with a masher at 800-1000 rpm to obtain 34 grams of finished catalyst, bottle it with nitrogen and seal it for use.

[0036] Preparation of polyglycerol:

[0037] Add 150 grams of glycerin in the 250mL four-neck flask with ...

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PUM

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Abstract

The invention discloses a preparation method used for preparing a catalyst of polyglycerol and application thereof, belonging to the technical filed of catalysts. The catalyst comprises at least a super basic material with alkali strength larger than 26 and a reductive phosphoric material. The preparation method comprises the following steps of taking gamma-Al2O3 as a carrier, dipping in a super-alkali solution, roasting, reacting with metallic Na for preparing the super basic material, and then mixing with the reductive phosphoric material to obtain the catalyst. The catalyst is used for polymerization reaction of glycerol and preparing the polyglycerol with light color and polymerization degree ranging from 2-20, and has the advantages of high catalytic activity, short reaction time, and high application value.

Description

technical field [0001] The invention belongs to a preparation method and application of a catalyst composition, in particular to a preparation method and application of a catalyst used for glycerin polymerization to prepare polyglycerol, and belongs to the technical field of catalysts. Background technique [0002] Polyglycerol belongs to polyhydroxy ether organic compounds, which can be used as humectants, tackifiers, plasticizers and hydrophilic modifiers, and is also an intermediate for the preparation of polyglycerol fatty acid ester surfactants. Polyglycerol is formed by intermolecular polymerization of glycerol or glycidol under the action of heating and catalysts. As far as the industrial preparation of polyglycerol is concerned, the following methods are known: [0003] (1) A method of recovering from the distillation residue of glycerin. [0004] (2) The method of dehydration polymerization with glycerol under the action of a catalyst. [0005] (3) Direct polymeri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/232B01J27/18C07C43/13C07C41/09C08G65/34
Inventor 刘学民王松营宋聪王祎
Owner JIANGNAN UNIV
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