Preparation method of crosslinked polystyrene-immobilized benzothiazole catalyst used for formose reaction

A cross-linked polystyrene and benzothiazole technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of non-recyclable and mechanically difficult product separation , uneven mass transfer and other problems, to achieve the effect of easy recycling, easy operation of reaction, and uniform mass transfer

Inactive Publication Date: 2013-09-18
SHANDONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, BETZB has the following disadvantages: it has a high boiling point, it is difficult to separate it from the product by simple methods, and it cannot be recycled and applied mechanically; when it is used as a catalyst for formose reaction in a rectifying tower or a fixed bed, the mass transfer is not uniform

Method used

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  • Preparation method of crosslinked polystyrene-immobilized benzothiazole catalyst used for formose reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of BE-PS:

[0032] Weigh 7g (66.6mmol) of cross-linked polystyrene (cross-linking degree 4%) after long-term low-temperature drying (drying temperature 60°C, drying time 10h), add it to 40ml 1,2-dichloroethane In the three-necked flask, swell at room temperature for 2h, then add 4g of anhydrous AlCl to the three-necked flask 3 , and slowly add 60g of 1,2-dibromoethane dropwise, and stir the reaction at 50°C for 20h, then stop the reaction, cool to room temperature, and then use ethanol, CCl 4 , washed with distilled water, and then dried at 60°C for 10 hours to obtain bromoethylated cross-linked polystyrene (BE-PS). The content of bromine atoms measured by the Volhard method is 17.65% (mass fraction), 2.21mmol / g (the number of moles of bromine atoms per gram of BE-PS).

[0033] (2) Preparation of BETZB-PS:

[0034] Weigh 7g of BE-PS, add it to a three-necked flask containing 30ml of 1,2-dichloroethane, add 10g of benzothiazole, reflux for 24 hours, co...

Embodiment 2

[0038] (1) Preparation of BE-PS:

[0039] Weigh 7g (66.6mmol) of cross-linked polystyrene (cross-linking degree: 2.5%) after long-term low-temperature drying (drying temperature 60°C, drying time 10h), add to 40ml 1,2-dichloroethane In a three-necked flask, swell at room temperature for 2h, and then add 2g of anhydrous AlCl to the three-necked flask 3 , and slowly dropwise added 40g of 1,2-dibromoethane, stirred at 50°C for 15h, stopped the reaction, cooled to room temperature, followed by ethanol, CCl 4 , washed with distilled water, and then dried at 60°C for 10 hours to obtain bromoethylated cross-linked polystyrene (BE-PS). The content of bromine atoms measured by the Volhard method was 11.08% (mass fraction), 1.39mmol / g.

[0040] (2) Preparation of BETZB-PS:

[0041] Weigh 7g of BE-PS, add it into a three-necked flask containing 40ml of 1,2-dichloroethane, add 10g of benzothiazole, reflux for 40h, cool to room temperature after the reaction, and use 1,2-dichloroethane ...

Embodiment 3

[0043] (1) Preparation of BE-PS:

[0044] Weigh 7g (66.6mmol) of cross-linked polystyrene (cross-linking degree: 7%) after long-term low-temperature drying (drying temperature 60°C, drying time 10h), add to 40ml 1,2-dichloroethane In the three-necked flask, swell at room temperature for 2h, then add 4g of anhydrous AlCl to the three-necked flask 3 , and slowly add 40g of 1,2-dibromoethane dropwise, and stir the reaction at 40°C for 20h, then stop the reaction, cool to room temperature, and then use ethanol, CCl 4, washed with distilled water, and then dried at 60°C for 10 hours to obtain bromoethylated cross-linked polystyrene (BE-PS). The content of bromine atoms measured by the Volhard method is 13.93% (mass fraction), 1.74mmol / g (the number of moles of bromine atoms per gram of BE-PS).

[0045] (2) Preparation of BETZB-PS:

[0046] Weigh 7g of BE-PS, add it to a three-necked flask containing 40ml of 1,2-dichloroethane, add 5g of benzothiazole, reflux for 15h, cool to roo...

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Abstract

The invention relates to a preparation method of crosslinked polystyrene-immobilized benzothiazole catalyst used for formose reaction. The method comprises the following steps of: (1) under the catalytic action of Lewis acid, carrying out alkylation reaction on the swelled crosslinked polystyrene and 1,2-dibromoethane to obtain bromoethyl crosslinked polystyrene (BE-PS for short); and (2) under the solvent reflux state, enabling the BE-PS to react with benzothiazole to obtain crosslinked polystyrene-immobilized benzothiazole (BETZB-PS for short). With the immobilized catalyst BETZB-PS synthesized by using the method, the technical defects that the traditional homogeneous catalyst is not applicable to a stationary bed and a rectifying tower for formose reaction, is difficultly separated from the product, not easy to recover and or reuse and the like can be overcome.

Description

technical field [0001] The invention relates to a preparation method of a cross-linked polystyrene immobilized benzothiazole catalyst for formose reaction. Background technique [0002] Formaldehyde sugar method, that is, the reaction method in which formaldehyde generates sugars and their analogs in the presence of alkali, the biggest advantage of this method is that the raw material is simple and easy-to-obtain formaldehyde, which has a significant competitive advantage economically; the hydroxyl group in its product Acetone (abbreviated as DHA) has a wide range of uses in chemical, pharmaceutical, cosmetic and food industries, etc., and its price is expensive, with great profit margins and market potential. [0003] Thiazole or benzothiazole onium salt catalyst is the newest catalyst for formose reaction. Under the optimal process conditions, the formaldehyde conversion rate and product selectivity can reach more than 90%, so that the formaldehyde technology can be devel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C49/17C07C45/45
Inventor 王志亮王伟萍
Owner SHANDONG UNIV OF SCI & TECH
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