Preparation method of fiber surface layer immobilized multistage phase transfer catalyst

A phase-transfer catalyst and fiber technology, which is applied in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc., to achieve the effects of not easy to break, long links, and easy control of process conditions

Inactive Publication Date: 2018-02-09
HENAN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Common synthetic fibers such as acrylic fibers have many excellent properties, but there are no reports on using them as carriers to prepare solid-supported phase transfer catalysts and then apply them in organic synthesis.

Method used

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  • Preparation method of fiber surface layer immobilized multistage phase transfer catalyst
  • Preparation method of fiber surface layer immobilized multistage phase transfer catalyst
  • Preparation method of fiber surface layer immobilized multistage phase transfer catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Accurately weigh 30.0 g of polyethylene polyamine in a three-necked flask, add equal mass of deionized water to stir and dilute evenly, heat to 105 °C under magnetic stirring, then weigh 3.0 g of dry acrylic fibrils, add In the above solution, the reaction was carried out at 105 °C for 24 h under reflux. Then take out the fiber, wash it with 60 ℃ deionized water until the pH value of the washing liquid is 7, dry it in the air, and then put it in a 60 ℃ electric heating constant temperature blast drying oven to vacuum dry to constant weight. chemical fiber PANF PSA . The reaction process is as figure 1 shown.

[0041] (2) Accurately weigh 10.0 g of ethyl bromide in a three-necked flask, add 100 mL of acetonitrile as a solvent, heat to reflux under stirring, and then put the dry PANF PSA Added to the above reaction solution, and kept under reflux for 8 h under magnetic stirring. Then cool to room temperature and take out the fiber, put it in 5% sodium carbonate ...

Embodiment 2

[0044] (1) The multi-level secondary amine surface functionalized fiber was prepared by the method in Example 1.

[0045] (2) Replace bromoethane with n-bromobutane of equal quality, press the method for embodiment 1, prepare the second kind of multilevel tertiary amine surface functionalized fiber PANF PTA -2. The reaction process is as Figure 4 shown.

[0046] (3) Replace benzyl bromide with n-bromobutane of equal mass, use PANF PTA -2 alternative to PANF PTA -1, by the method for embodiment 1, prepare the second kind of fiber surface immobilized multi-level quaternary ammonium salt PANF PQAB -2. The reaction process is as Figure 5 shown.

Embodiment 3

[0048] (1) The multi-level secondary amine surface functionalized fiber was prepared by the method in Example 1.

[0049] (2) By the method of Example 2, prepare the second multi-level tertiary amine surface functionalized fiber PANF PTA -2.

[0050] (3) Use PANF PTA -2 alternative to PANF PTA -1, according to the method of embodiment 1, prepare the third kind of fiber surface immobilized multi-stage quaternary ammonium salt PANF PQAB -3. The reaction process is as Image 6 shown.

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Abstract

The invention relates to a preparation method of a fiber surface layer immobilized multistage phase transfer catalyst. The preparation method comprises following steps: 1, multistage secondary amine surface functionalized fiber is synthesized via acrylic fiber water-phase ammonification; 2, the multistage secondary amine surface functionalized fiber and a halogenated hydrocarbon are subjected to first salt forming and neutralization so as to obtain a multistage tertiary amine surface layer functional fiber; and 3, the multistage tertiary amine surface layer functional fiber and the halogenatedhydrocarbon are subjected to secondary salt forming so as to obtain the fiber surface layer immobilized multistage phase transfer catalyst which is high in supported quantity, excellent in active sites, and excellent in catalytic effect and stability, and is convenient to be recycled. The fiber surface layer immobilized multistage phase transfer catalyst is high in mechanical strength, and possesses excellent secondary processing performance, can be prepared into different needed shapes for different fixed bed reactors via weaving, and a novel approach is provided for novel continuous industrialized catalysis.

Description

technical field [0001] The invention belongs to the technical field of green catalysis, and relates to a preparation method of a multi-level phase transfer catalyst immobilized on the surface of fibers. Background technique [0002] In recent years, resource and environmental problems have become more and more serious. As the frontier of international chemical science research, green chemistry has attracted widespread attention from scientists around the world. Its active exploration and attempts in many fields have played a significant role in the sustainable development of economy and society. Significant impetus has been achieved. According to statistics, more than 85% of the chemical reaction process involves the use of catalysts, so the innovation of green catalytic technology has gradually attracted people's attention. Among them, the study of immobilizing the catalytically active components that are difficult to recover on carrier materials and carrying out immobiliz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06C07C315/00C07C331/04C07C317/18
Inventor 史显磊胡倩倩陈永菊段培高王枫
Owner HENAN POLYTECHNIC UNIV
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