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Silica microsphere-supported urea catalyst and its preparation method and application
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A technology of silica and catalyst, which is applied in the chemical industry, can solve the problems of polymer residues, etc., and achieve the effects of high recovery rate, improved stability, and mild reaction conditions
Active Publication Date: 2022-03-15
QINGDAO UNIV OF SCI & TECH
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[0006] The purpose of the present invention is to provide a silica microsphere-supported urea catalyst to solve the problem that the urea catalyst in the prior art has residues in the prepared polymer;
Method used
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Embodiment 1 2
[0053] The preparation method and application of embodiment 1 silica microsphere supported urea catalyst
[0054] The structure of the silica microsphere supported urea catalyst involved in this embodiment is as follows:
[0055]
[0056] Its preparation process is as follows:
[0057] 1) Preparation of aminopropylated silica microspheres
[0058] Weigh 5.0kg of silicon dioxide and 1.5kg of 3-aminopropyltriethoxysilane (hereinafter referred to as KH550) and add them to 50L of toluene, then add 3.5L of water, stir and react at 25°C for 2h, filter, and wash with water (3L×3 ), and then dried at 100° C. for 3 h to obtain 5.4 kg of aminopropylated silica microspheres.
[0059] The chemical reaction formula of this preparation process is as follows:
[0060]
[0061]2) Preparation of silica microsphere-supported urea catalyst
[0062] Under nitrogen protection, weigh 1 kg (1 mol) of aminopropylated silica microspheres and place them in a reactor, vacuum-dry them at 50°C f...
Embodiment 2-14 2
[0070] Example 2-14 Preparation method and application of silica microsphere-supported urea catalyst
[0071] Examples 2-14 are respectively a preparation method and application of a silica microsphere-supported urea catalyst, and their steps are basically the same as in Example 1, except that the preparation method and various process parameters during application are different, See Table 1 and Table 2 for details:
[0072] List of each technological parameter in the embodiment 2-7 of table 1
[0073]
[0074]
[0075]
Embodiment 2
[0076] The structure of the silica microsphere supported urea catalyst involved in embodiment 2 is as follows:
[0077]
[0078] SiO 2 -U2 detection:
[0079] The prepared SiO 2 -U2 for detection by infrared spectroscopy. The result is displayed at 1092cm -1 The characteristic absorption peak of Si-O bond appears at 1655cm -1 and 1505cm -1 The characteristic absorption peak of the urea carbonyl group appears.
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Abstract
The invention belongs to the field of chemical industry, and discloses a silica microsphere-supported urea catalyst and a preparation method thereof. It is prepared after reaction; the invention also discloses an application of the above-mentioned silicon dioxide microsphere-supported urea catalyst and an organic base synergistically catalyzing the ring-opening polymerization of lactone monomers. The silica microsphere-supported urea catalyst provided by the present invention can be separated from the reactants by simple filtration, ensuring that there is no urea catalyst residue in the polymer, and the number average molecular weight of the polymer is controlled between 1000-100000g / mol, The molecular weight distribution is narrow, which solves the problem that the urea catalyst remains in the prepared polymer in the prior art. The silicon dioxide microsphere-supported urea catalyst of the invention is suitable for use as a catalytic system in cooperation with an organic base in the process of preparing a polymer from a lactone monomer.
Description
technical field [0001] The invention belongs to the field of chemical industry and relates to a catalyst, in particular to a silica microsphere-loaded urea catalyst and its preparation method and application. Background technique [0002] The increasing popularity of plastic products not only brings convenience to human life, but also causes huge damage to the ecological environment. White pollution has become an urgent problem to be solved, and the use of degradable materials is one of the important means to solve white pollution. Aliphatic polyesters are an excellent class of degradable materials, which can be prepared by polycondensation of lactic acid, etc., or by ring-opening polymerization of lactone monomers. Its degradability and human compatibility make it have good prospects and markets in industries such as medical and health care, agriculture, aquatic products, and food packaging. [0003] Waymouth et al disclosed in "Organocatalytic Ring Opening Polymerization...
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