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Cyclic oligomeric phosphazene base catalyst loaded on polystyrene microspheres and its preparation method and use

A technology of polystyrene microspheres and polystyrene, applied in the field of organic chemistry, can solve the problems of limited catalyst types, complex synthesis methods, and high cost

Active Publication Date: 2021-07-16
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Although phosphazene compounds have been studied for many years, the types of common phosphazene compound catalysts are limited, the synthesis method is complicated, and the cost is high, which is not conducive to the application of large-scale production.

Method used

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  • Cyclic oligomeric phosphazene base catalyst loaded on polystyrene microspheres and its preparation method and use
  • Cyclic oligomeric phosphazene base catalyst loaded on polystyrene microspheres and its preparation method and use
  • Cyclic oligomeric phosphazene base catalyst loaded on polystyrene microspheres and its preparation method and use

Examples

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preparation example Construction

[0088] Preparation method of catalyst

[0089] In a second aspect of the invention, the present invention has proposed a method of preparing a catalyst of the above examples. According to an embodiment of the invention, the method comprises:

[0090] (1) The chloromethyl substituted polystyrene-divinylbenzene is a vacuum drying treatment. Specifically, the chloromethyl substituted polystyrene-divinylbenzene, which may be sufficiently washed with methanol before use, and then substituted with methanol-washed chloromethal-substituted polystyrene-divinyl group The beads of the beads were dried in vacuo at 50 ° C for 2 to 24 h.

[0091]According to an embodiment of the present invention, the chloromethyl substituted polystyrene-divinylbenzene-difinylbenzene can be 100 to 600 mesh, preferably 200 to 400 mesh.

[0092] According to an embodiment of the invention, the functional group density of the chloromethyl substituted polystyrene-divinylbenzene-di-diobenzene bead may be 1 to 4 mmol...

Embodiment 1

[0138] First step, preparation of aminocyreopyrene microspheres

[0139] Using methanol thorns 11 g of methyl chloromethyl substituted polystyrene-divinylbenzene multi-p-copolymer bead (1% DVB, 200 ~ 400 mesh, 1 to 1.3 mmol cl / g), 50 ° C, vacuum drying 24 hours . Under a nitrogen atmosphere, anhydrous tetrahydrofuran (THF) was added to allow the copolymer beads for 24 hours, separated from the solid, dried in vacuo at 50 ° C for 24 hours.

[0140] 10 g of pre-treated chloromethyl polystyrene microspheres were placed in 150 ml N, N-dimethylformamide (DMF), added (3.4 g, 17.8 mmol) of phthalimide potassium, at 50 Stir at ° C for 24 hours. After the reaction, the tan polymer bead was filtered. DMF (20 mL × 3), methanol (20 ml × 3), and methanol (20 mL × 5) were washed again. The resulting polymer was dried in vacuo at 50 ° C for 24 hours, weighed 11.8 g.

[0141] The above-mentioned brown polymer 11.8 g was added to anhydrous ethanol, 2 ml of hydrated compound, and refluxed for 24 ...

Embodiment 2

[0148] First step, the preparation of aminocyreolystyrene microspheres is the same as in Example 1

[0149] Step 2, three [three (diethylamine) phosphorus nitrocene] Preparation of trichloropathic acid

[0150] Phalochloride (20.9 g, 0.1 mol) was added to a three-mouth flask equipped with mechanical stirring, and 75 ml of anhydrous methylene chloride was added under a nitrogen protection, which was placed in a low-temperature bath of -40 ° C to maintain vigorous stirring. Dietamine (62 mL, 0.6 mol) was added dropwise to the reaction system, and the temperature of the solution was lower than -30 ° C. After passing, the temperature is naturally raised to 20 ° C and the reaction is continued for 2 hours. The system temperature was again reduced to 0 ° C, and the ammonia gas was accented to saturation, raised to 20 ° C, and the ammonia gas was continued for 3 hours until the stirring surface did not precipitate. The solvent was filtered off, and the solvent was evaporated under reduce...

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Abstract

The invention discloses a cyclic oligomeric phosphazene base catalyst loaded on polystyrene microspheres, a preparation method and application thereof. The catalyst supports the cyclic oligomeric phosphazene base on the polystyrene microsphere carrier through chemical bonding, which can effectively avoid the detachment of the catalytic active center during use, and the catalyst can be separated from the polymerization reaction product by simple filtration , and repeated use can still maintain high catalytic activity, while containing no metal elements, good environmental benefits.

Description

Technical field [0001] The present invention relates to the field of organic chemistry, and in particular, the present invention relates to a cyclic oligo-phosphorne catalyst loaded in polyphenylene microspheres and a preparation method thereof. Background technique [0002] Phosphate nitrile is a type of non-polar strong alkaline compound containing a P = N bond, including phosphate nitrile, phosphazene, and phosphate nitrile. Among them, phosphoricercine has superior alkaline, weak priests and has good solubility in most solvents. The above advantages can significantly increase the activity of the phosphorite catalytic open loop polymerization reaction, and can effectively solve the metal residue of the catalyst in the polyether and polyester. The phosphonitrile catalyst is widely used in an anionic open loop polymerization reaction of a cyclic monomer, including an epoxy monomer, a cyclosiloxane, lactam, cycloalkyl, cycloalk carbonate, and the like. The current research is con...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08G63/87C08G63/08C08G77/08C08F120/14C08F4/02C08F4/00C08F120/56C08G69/14
CPCC08F4/00C08F4/027C08F120/14C08F120/56C08G63/08C08G63/823C08G63/87C08G65/2612C08G69/14C08G77/08
Inventor 李志波任传利赵娜付小会刘绍峰
Owner QINGDAO UNIV OF SCI & TECH
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