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Preparation method of crosslinked polystyrene microsphere surface synthesized 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: 2015-11-25
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

But, in the research of current NHPI catalytic oxidation system, used NHPI is homogeneous catalyst (ToribioPP, Gimeno-GargalloA, Capel-SanchezMC, deFrutosMP, Campos-MartinJM, FierroJLG.AppliedCatalysisA:General,2009,363:32 ), obviously there are problems such as the catalyst is not easy to separate and reuse and the system is not easy to purify

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

Embodiment 2

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

Embodiment 3

[0018] In a four-neck flask, soak 0.5g CMCPS microspheres (17% chlorine) in 30mL DMF and Dioxane mixed solvent (V:V=1:1) for swelling for 13 hours, add 1.6gTMA, 0.6mL triethylamine. Constant temperature at 100°C, stirring and reacting for 6.5h, suction filtration, washing with a mixed solvent of DMF and Dioxane and anhydrous ether, and vacuum drying to constant weight to obtain the modified microstructure with phthalic anhydride (PA) bonded on the surface Ball CPS-PA. Soak 1g of modified microspheres CPS-PA in 30mL of anhydrous pyridine to swell for 13h, then add 1.4g of hydroxylamine hydrochloride, react for 12h under constant temperature stirring at 75°C, cool, acidify with hydrochloric acid, filter, wash the microspheres repeatedly with distilled water, and dry in vacuum 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 2.3mmol / g.

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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 specifically relates to a method for synthesizing and immobilizing N-hydroxyphthalimide on the surface of cross-linked polystyrene microspheres. Process for the preparation of amine catalysts. Background technique [0002] The transformation of hydrocarbons into oxygenates and alcohols into deep oxides plays an extremely important role in the chemical industry. However, the traditional oxidation process generally uses stoichiometric strong inorganic oxidants, which brings serious environmental problems. From the perspective of green and sustainable chemistry, catalytic oxidation using oxygen or atmospheric oxygen as an oxygen source is a clean and economical organic synthesis route, which has been vigorously researched and developed in recent years. Using molecular oxygen to realize the oxidative transformation of org...

Claims

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Application Information

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