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A kind of preparation method of cross-linked polystyrene microsphere surface synthesis and immobilized n-hydroxyphthalimide catalyst

A technology of hydroxyphthalimide and cross-linked polystyrene, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, carbon-based compound preparation, etc., can solve the problem of difficult purification of the system , Catalysts are not easy to separate and reuse, etc., to achieve the effect of easy purification of the system, good catalytic activity, and convenient treatment

Active Publication Date: 2017-09-05
铁居科技(海南)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the current research on NHPI catalytic oxidation system, the NHPI used are all homogeneous catalysts (Toribio P P, Gimeno-Gargallo A, Capel-Sanchez M C, de Frutos M P, Campos-Martin J M, Fierro J L G. Applied Catalysis A: General, 2009, 363:32), obviously there are problems such as difficult separation and reuse of the catalyst and difficult purification of the system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] In a four-necked bottle, soak 0.5g of CMCPS microspheres (12% chlorine content) in 30mL of DMAC to swell for 12 hours, add 1.3g of TMA, and 0.5mL of triethylamine. Constant temperature at 110 °C, stirring and reacting for 6.5 h, suction filtration, washing with DMAC and anhydrous ether, and vacuum drying to constant weight to obtain modified microspheres CPS-PA with phthalic anhydride (PA) bonded on the surface. Immerse 1g of modified microspheres CPS-PA in 30mL of anhydrous pyridine to swell for 12h, then add 0.8g of hydroxylamine hydrochloride, react under constant temperature stirring at 90°C for 15h, cool, acidify with hydrochloric acid, filter, repeatedly wash the microspheres with distilled water, and vacuum dry To a constant weight, the polymer microspheres CPS-NHPI with N-hydroxyphthalimide (NHPI) immobilized on the surface were obtained, and the immobilized amount of NHPI was 2.3 mmol / g.

Embodiment 2

[0016] In a four-necked bottle, soak 0.5g of CMCPS microspheres (14% chlorine content) in 30mL of DMF to swell for 14 hours, add 1.13g of TMA and 0.49mL of triethylamine. Constant temperature at 105°C, stirring and reacting for 6h, suction filtration, washing with DMF and anhydrous ether, and vacuum drying to constant weight to obtain modified microspheres CPS-PA with phthalic anhydride (PA) bonded on the surface. Immerse 1 g of modified microspheres CPS-PA in 30 mL of anhydrous pyridine to swell for 14 hours, then add 0.78 g of hydroxylamine hydrochloride, react under constant temperature stirring at 80 °C for 18 hours, cool, acidify with hydrochloric acid, filter, repeatedly wash the microspheres with distilled water, and vacuum dry To a constant weight, the polymer microspheres CPS-NHPI with N-hydroxyphthalimide (NHPI) immobilized on the surface were obtained, and the immobilized amount of NHPI was 2.35 mmol / g.

Embodiment 3

[0018] In a four-necked bottle, soak 0.5g of CMCPS microspheres (containing 17% chlorine) in 30mL of a mixed solvent of DMF and Dioxane (V:V=1:1) to swell for 13 hours, add 1.6g of TMA, 0.6mL of three Ethylamine. Constant temperature at 100 °C, stirring and reacting for 6.5 h, suction filtration, washing with a mixed solvent of DMF and Dioxane and anhydrous diethyl ether, and vacuum drying to constant weight to obtain a modified microparticle with phthalic anhydride (PA) bound on the surface. Ball CPS-PA. Immerse 1g of modified microspheres CPS-PA in 30mL of anhydrous pyridine to swell for 13h, then add 1.4g of hydroxylamine hydrochloride, react under constant temperature stirring at 75°C for 12h, cool, acidify with hydrochloric acid, filter, repeatedly wash the microspheres with distilled water, and vacuum dry To a constant weight, the polymer microspheres CPS-NHPI with N-hydroxyphthalimide (NHPI) immobilized on the surface were obtained, and the immobilized amount of NHPI w...

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Abstract

The invention belongs to the technical field of a polymeric microsphere surface immobilized N-hydroxyphthalimide catalyst and specifically relates to a preparation method of a crosslinked polystyrene microsphere surface synthesized and immobilized N-hydroxyphthalimide catalyst. According to the preparation method, chloromethylated crosslinked polystyrene microspheres CMCPS are immersed in a de-watering solvent to undergo swelling so as to prepare modified microspheres CPS-PA with the surface bonded with phthalic anhydride; and then, the modified microspheres CPS-PA with the surface bonded with phthalic anhydride is used to prepare crosslinked polystyrene microsphere surface synthesized and immobilized N-hydroxyphthalimide. The method provided by the invention has advantages as follows: good stability, simple process, convenience in operation and high immobilization capacity. The product is easy to separate in a catalytic oxidation system and has good reusability, and the system is easy for purification.

Description

technical field [0001] The invention belongs to the technical field of N-hydroxyphthalimide catalysts immobilized on the surface of polymer microspheres, and in particular relates to the synthesis of cross-linked polystyrene microspheres and the immobilization of N-hydroxyphthalimide on the surface Preparation method of amine catalyst. Background technique [0002] The transformation of hydrocarbons into oxygenates and alcohols into deep oxides play an extremely important role in the chemical industry. However, the traditional oxidation process generally uses a stoichiometric amount of inorganic strong oxidants, which brings serious environmental problems. From the viewpoint of green and sustainable chemistry, catalytic oxidation using oxygen or air oxygen as oxygen source is a clean and economical route for organic synthesis, which has been vigorously researched and developed in recent years. Molecular oxygen is used to realize the oxidative transformation of organic comp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/06B01J35/08C08F12/08C08F8/32C08F8/00C07C51/265C07C63/06C07C45/39
Inventor 杜瑞奎门吉英高保娇王蕊欣黄建龙
Owner 铁居科技(海南)有限公司
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