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Method for preparing beta-ionone epoxidation catalyst from wheat straw

A technology for ionone rings and oxidation catalysts, which is applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., and can solve material quality loss, selenium loss, resource waste, etc. problem, to achieve strong catalytic activity, good application value, and simple catalyst process

Active Publication Date: 2019-09-13
YANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since the dehydration carbonization process of sugars needs to be calcined at high temperature, in this process, the mass loss of substances is serious, including a certain amount of selenium loss, which can cause a certain waste of resources

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Catalyst synthesis: Add 100 mL of ethanol solution of sodium selenium hydride (0.01 mol / L, prepared on site from selenium powder and sodium borohydride, 1 mmol) in a 500 mL round bottom flask, add 13 g of wheat straw dry powder at one time while stirring (prepared by drying wheat straw, crushing it, and then drying it, with a water content of less than 3%), adding 0.4mmol 2-trifluorosilyloxyethanol (CF 3 SiOCH 2 CH 2 OH, 0.1mol / L ethanol solution, take 4 mL), 20 o After stirring at C for 24 hours, the solid was filtered and dried, which was the catalyst material.

[0018] Catalyst activity characterization: 30 mg of the catalyst material, 1 mL of β-ionone in ethyl acetate (1 mol / L), 1 mL of H 2 o 2 Acetonitrile solution (by 30% H 2 o 2 Prepared with acetonitrile, concentration 1mol / L), 80 o C was heated for 24 hours, the solvent was evaporated to dryness, and the residue was separated by preparative thin-layer chromatography (petroleum ether: ethyl acetate 10:1 ...

Embodiment 2

[0020] Other conditions are the same as in Example 1, and the properties of the materials synthesized by using different fluorine-containing additives are tested, and the experimental results are shown in Table 1.

[0021] Table 1 Performance comparison of materials synthesized using different fluorine-containing additives

[0022] serial number Fluorinated additives Yield of β-ionone epoxidation reaction (%) 1 2-Trifluorosilyloxyethanol 71 (Example 1) 2 3-Trifluorosilyloxypropanol 52 3 Trifluorosilyloxymethanol 32 4 2-fluoroethanol 22 5 ammonium fluoride 17 6 Tetra-n-butylammonium fluoride 23 7 Trifluoroacetate 14

[0023] From the above results, it can be seen that the catalytic performance of the material prepared by using 2-trifluorosiloxyethanol (Example 1) is the best.

Embodiment 3

[0025] Other conditions were the same as in Example 1, and the effects of using different ratios of wheat straw dry powder and sodium selenium hydride were tested, and the experimental results are shown in Table 2.

[0026] Table 2 Effect comparison table of different wheat straw dry powder and sodium selenium hydride usage ratio

[0027] serial number Ratio of wheat straw dry powder and sodium selenium hydride Yield of β-ionone epoxidation reaction (%) 1 10g: 1mmol 40 2 11g: 1mmol 52 3 12g: 1mmol 66 4 13g: 1mmol (Example 1) 71 5 14g: 1mmol 68 6 15g: 1mmol 62 7 16g: 1mmol 55

[0028] From the above results, it can be known that the ratio of wheat straw dry powder to sodium selenium hydride is 13g:1mmol, and the prepared material has the highest catalytic activity (Example 1).

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PUM

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Abstract

The invention discloses a method for preparing a beta-ionone epoxidation catalyst from wheat straw. The preparation method comprises the following steps: uniformly mixing wheat straw dry powder with sodium selenide according to a ratio of 10-16 g: 1 mmol, adding 2-trifluorosiloxyethanol with a molar weight of 0.3-0.5 times of sodium selenide, carrying out stirring for 24 hours at a temperature of10-30 DEG C, and then filtering and drying the solid to obtain the catalyst material. The material has high catalytic activity and can catalyze a selective epoxidation reaction of beta-ionone.

Description

technical field [0001] The invention relates to a method for preparing a β-ionone selective epoxidation catalyst by selenization of wheat straw dry powder, belonging to the field of catalytic material preparation. Background technique [0002] Selenium-catalyzed chemistry is a new field emerging in recent years. my country is rich in selenium resources, and the development of new application methods for selenium can give full play to our country's unique resource advantages and conform to the characteristics of our country's resources. Selenium can be metabolized by organisms and will not be deposited in the body, so it is friendly to the environment. The reaction catalyzed by selenium usually uses a green and clean oxidant, the reaction process is environmentally friendly, and has good industrial application value. [0003] However, most of the selenium-catalyzed reactions reported so far use homogeneous selenium catalysts, which are difficult to recycle, thus increasing ...

Claims

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Application Information

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IPC IPC(8): B01J31/02C07D303/32
CPCB01J31/0275B01J2231/72C07D303/32
Inventor 俞磊杨钰帆刘闯
Owner YANGZHOU UNIV
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