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Preparation method of dipropylene glycol and catalyst thereof

A dipropylene glycol reduction and catalyst technology, which is applied in the direction of physical/chemical process catalysts, ether preparation, organic compounds/hydrides/coordination complex catalysts, etc., can solve problems such as corrosion equipment, polluted environment treatment, difficulties, etc., and achieve easy Recycling, high catalytic activity, mild effect

Pending Publication Date: 2021-08-27
ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention is based on at least one of the above technical problems. The conditions of the present invention are mild, and the catalyst is composed of nucleophilic ions and cyclodextrin compounded on hydrotalcite. It is non-polluting, easy to synthesize, easy to recycle and can be reused. High-quality DPG can be synthesized as a reactant, which overcomes a series of shortcomings such as corrosion equipment, environmental pollution and subsequent processing difficulties in the traditional method of preparing DPG.

Method used

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  • Preparation method of dipropylene glycol and catalyst thereof
  • Preparation method of dipropylene glycol and catalyst thereof
  • Preparation method of dipropylene glycol and catalyst thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Specific Preparation of Heterogeneous Catalysts

[0032] (1) Preparation of Al-Mg hydrotalcite

[0033] The preparation method of the aluminum-magnesium hydrotalcite is as follows: the precursor aluminum-magnesium hydrotalcite with good crystallinity is synthesized by a hydrothermal uniform precipitation (urea hydrolysis) method. The experimental procedure is: take 12.82g of Mg(NO 3 ) 2 •6H 2 O, 9.38g of Al(NO 3 ) 3 •9H 2 O and 7.36g of urea are made into a mixed solution, wherein Mg 2+ : 0.1mol / L, Al 3+ : 0.05mol / L, urea: 0.245mol / L. Then take 50mL of the mixed solution and add it to a 100mL hydrothermal reaction kettle, and react at 140°C for 24 hours to obtain a white precipitate, which is washed with a large amount of distilled water, filtered with suction, and the obtained aluminum-magnesium hydrotalcite sample is dried in the air.

[0034](2) Preparation of nucleophilic ion and cyclodextrin compound

[0035] Calcining the aluminum-magnesium hydrotalcite ...

Embodiment 2

[0037] Specific Preparation of Heterogeneous Catalysts

[0038] (1) Preparation of Al-Mg hydrotalcite

[0039] This part of technical feature is identical with embodiment 1.

[0040] (2) Preparation of nucleophilic ion and cyclodextrin compound

[0041] Al-Mg hydrotalcite was calcined at 600°C for 3 hours to obtain Al-Mg oxide. The bromide ion is inserted into the hydrotalcite by utilizing the property of hydrotalcite calcining reduction. At the same time, cyclodextrin and hydrotalcite are combined to obtain a new type of composite material. The experimental steps are: use 0.973g of α-cyclodextrin to dissolve into 50 ml of carbon dioxide-free distilled water and add 0.2g of KBr, and add 0.2g of Al-MgO, and stirred at 60° C. for 24 hours under nitrogen protection. Suction filtration at room temperature and washing with a large amount of carbon dioxide-free distilled water to obtain a white solid, which was vacuum-dried at 80° C. for 10 h. The obtained heterogeneous catalys...

Embodiment 3

[0043] Specific Preparation of Heterogeneous Catalysts

[0044] This part of technical feature is identical with embodiment 1.

[0045] (2) Preparation of nucleophilic ion and cyclodextrin compound

[0046] A certain amount of aluminum-magnesium hydrotalcite is calcined at 400° C. for 4 hours to obtain aluminum-magnesium oxide. The bromide ion is inserted into the hydrotalcite by utilizing the property of hydrotalcite calcining reduction. At the same time, cyclodextrin and hydrotalcite are combined to obtain a new type of composite material. The experimental steps are: use 1.134g of β-cyclodextrin to dissolve into 50 ml of carbon dioxide-free distilled water and add 0.2g of KBr, and add 0.2g of Al-Mg oxide, and stirred at 2.0 Mpa at 80° C. for 24 hours under a nitrogen protection environment. Suction filtration at room temperature and washing with a large amount of carbon dioxide-free distilled water to obtain a white solid, which was vacuum-dried at 60° C. for 12 h.

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Abstract

The invention provides a preparation method of dipropylene glycol and a catalyst thereof. The catalyst is prepared by loading nucleophilic ions and cyclodextrin on aluminum-magnesium hydrotalcite. The nucleophilic ions are bromide ions; and the cyclodextrin is alpha-cyclodextrin, gamma-cyclodextrin or beta-cyclodextrin. According to the method, the conditions are mild, the catalyst is formed by compounding nucleophilic ions and cyclodextrin on hydrotalcite, pollution is avoided, synthesis is easy, recycling is easy, the high-quality DPG can be synthesized by using the epoxy compound as a reactant, and a series of defects that equipment is corroded, the environment is polluted, follow-up treatment is difficult and the like in a traditional method for preparing the DPG are overcome.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of dipropylene glycol and a catalyst thereof. Background technique [0002] Propylene glycol oligomers are an important class of organic chemical products, especially dipropylene glycol (DPG) is more widely used. Dipropylene glycol (DPG) is a colorless, odorless liquid at room temperature, non-corrosive Sex, little irritation to skin, very low toxicity, widely used. Dipropylene glycol is divided into LO+ grade and industrial grade. The former is relatively expensive, and is mainly used in fields requiring high-quality raw materials such as spices, cosmetics, detergents, and food additives; the latter is relatively low in price, and is widely used as an industrial solvent that does not require high DPG quality and as a solvent for unsaturated polyester. Raw materials for production, nitrocellulose varnish, etc. [0003] At present, in the industr...

Claims

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Application Information

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IPC IPC(8): B01J31/06C07C41/02C07C43/13
CPCB01J31/065B01J31/069C07C41/02C07C43/132
Inventor 张智强王国庆徐浩洋绪连彩陈俊利
Owner ZHENGZHOU UNIVERSITY OF LIGHT INDUSTRY
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