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Load type carbon nano-fiber catalyst and application thereof

A carbon nanofiber, supported technology, applied in the field of green synthesis of styrene cyclic carbonate, can solve the problems of loss of gold elements, uneconomical availability of raw materials, reduced conversion rate and selectivity, etc., and achieves low production cost. , The engineering conditions are reasonable and easy to control, and the reaction yield is high.

Inactive Publication Date: 2011-08-03
WENZHOU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] But it is clear that in this technology, Au / SiO 2 and Au / Fe(OH) 3 The raw materials for catalyst preparation are not economical and easy to obtain, and Au / Fe(OH) 3 The preparation process must strictly control the pH of the system, repeatedly wash to remove chloride ions, and roast at a certain temperature.
And due to the loss of gold element, when the recovered catalyst is used for catalytic oxidation again, the conversion rate and selectivity of the reaction are both reduced.

Method used

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  • Load type carbon nano-fiber catalyst and application thereof
  • Load type carbon nano-fiber catalyst and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Embodiment 1: the preparation of acetylacetonate vanadyl complex

[0030] Put 36.4g of vanadium pentoxide solid and equimolar acetylacetone in a three-necked flask to reflux for 20 hours, filter the suspension while hot, wash the solid product with acetone and ether, and dry at 110°C to obtain the green product vanadyl acetylacetonate complex [VO(C 5 h 7o 2 ) 2 ] (molecular weight 265.16).

Embodiment 2

[0031] Embodiment 2: the preparation of nickel acetylacetonate complex

[0032] 59.4g NiCl 2 .6H 2 O was dissolved in 150 mL of water (C solution), and 50 g of acetylacetone (0.5 mol) was dissolved in 100 mL of methanol (D solution). Add C to D and stir, then add 150 mL of aqueous solution containing 0.5 mol of sodium acetate (molecular weight: 136.08). The above mixture was reacted for 5 hours, kept in the refrigerator for several hours, filtered the green solid, washed with water, and dried at 110°C to obtain the nickel acetylacetonate complex [Ni(C 5 h 7 o 2 ) 2 ] (molecular weight 256.91).

Embodiment 3

[0033] Embodiment 3: surface oxidation treatment of carbon nanofibers

[0034] In a PTFE-lined autoclave, a mixture of concentrated nitric acid and concentrated sulfuric acid (volume ratio: 5:4) was used as an oxidant to treat CNF at 90 °C with constant temperature stirring for 1 h, and then it was washed with water, filtered and dried at 120 °C. overnight. The treated samples were designated as CNF90.

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Abstract

The invention discloses a load type carbon nano-fiber catalyst and application thereof. The catalyst is obtained by grafting a metal complex of acetylacetone to carbon nano-fiber undergoing the surface oxidation treatment; and the metal complex of acetylacetone is vanadyl acetylacetone or nickel acetylacetone. When the load type carbon nano-fiber catalyst is used for synthesizing styrene cyclic carbonate ester, styrene and carbon dioxide used as raw materials react in a high-pressure reaction kettle in the presence of the load type carbon nano-fiber catalyst, tetrabutyl ammonium bromide, zincbromide and an oxidant at a temperature of between 80 and 120 DEG C and under a pressure of between 3 and 6.5Mpa to obtain the styrene cyclic carbonate ester. The catalyst has the advantages of thoroughly solving the problem of serious three-waste pollution existing in the prior art, facilitating the environmental protection, being easily and conveniently operated, having high reaction yield and low production cost, and having greater implementation and popularization values and social and economic benefits.

Description

(1) Technical field [0001] The invention relates to a supported carbon nanofiber catalyst and application thereof, and the application specifically relates to a green synthesis method of styrene cyclic carbonate. (2) Background technology [0002] Cyclic carbonates can be prepared by cycloaddition of alkylene oxide and carbon dioxide under the action of a catalyst. As an organic solvent with excellent performance, cyclic carbonates, especially styrene cyclic carbonates, are used in medicine and fine chemicals The synthesis of the product has a wide range of applications, so it has become a current research hotspot. [0003] In the early technology of synthesizing cyclic carbonates, toxic organic solvents must be added, and homogeneous organic base catalysts must be used to carry out under relatively high temperature and pressure. Therefore, there are disadvantages such as difficulty in catalyst separation, serious environmental pollution, and high production cost. In the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J35/06C07D317/36B01J31/22B01J21/18
Inventor 乔迁唐天地王如国
Owner WENZHOU UNIV
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