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A method for the joint preparation of styrene oxide and benzaldehyde using sio2-coo composite airgel as a catalyst

A technology of composite airgel and styrene oxide, which is applied in chemical instruments and methods, oxidation preparation of carbonyl compounds, physical/chemical process catalysts, etc. The reaction temperature is not easy to control and other problems, to achieve the effect of easy separation, obvious solvent effect and low requirements

Active Publication Date: 2016-05-25
HUAWEI TEHCHNOLOGIES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Benzaldehyde produced by traditional toluene chlorination and hydrolysis inevitably contains trace amounts of organic chlorine, which limits its application in pharmaceutical and spice industries
Patent CN1876616 produces benzaldehyde by benzoate reduction method. Although the single-pass conversion rate and benzaldehyde selectivity of this method are very high, the reaction temperature must be above 300°C, which requires high energy consumption and high raw material costs.
Patent CN1068755 discloses a method for preparing benzaldehyde by gas-phase oxidation of toluene. Although this method is economical and environmentally friendly, and the selectivity of benzaldehyde is as high as 99%, the single-pass conversion rate of toluene is only 26%.
In addition, the gas-phase oxidation reaction of toluene is a strong exothermic reaction, and the reaction temperature is difficult to control. When the temperature is too high, benzaldehyde is easily over-oxidized to produce a series of by-products such as benzoic acid and carbon dioxide. In order to control the reaction temperature, it is necessary to increase equipment investment

Method used

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  • A method for the joint preparation of styrene oxide and benzaldehyde using sio2-coo composite airgel as a catalyst
  • A method for the joint preparation of styrene oxide and benzaldehyde using sio2-coo composite airgel as a catalyst
  • A method for the joint preparation of styrene oxide and benzaldehyde using sio2-coo composite airgel as a catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-5

[0023] Examples 1-5: SiO with different n(Si / Co) 2 Combined preparation of styrene oxide and benzaldehyde by epoxidation of styrene catalyzed by -CoO composite airgel

[0024] Into five 50mL two-necked round bottom flasks, add 0.25g of catalysts prepared above with n(Si / Co) of 50, 100, 150, 200, 250, styrene 1.04g (10mmol), N,N-di Methylformamide 10g, the flask was reacted at a constant temperature in an oil bath at 60°C, refluxed for 6h, while stirring continuously, 10ml (10mmol) of 30% hydrogen peroxide was added at a constant speed by a micro-injection pump, and the dropping time was 0.5h. After the reaction, the catalyst was separated by filtration, and the filtrate was analyzed by gas chromatography. The filtrate was rectified, and the fractions at 180°C and 190°C were taken respectively to obtain styrene oxide and benzaldehyde in sequence. The product was qualitatively analyzed by GC-MS (CP-3800 / Saturn2000 gas / mass spectrometer, capillary column: CP-SIL8, 30m*0.25mm*0....

Embodiment example 6~9

[0028] Implementation Cases 6~9: SiO with Different Catalyst Consumption 2 -CoO Composite Airgel Catalyzed Epoxidation of Styrene to Jointly Prepare Styrene Oxide and Benzaldehyde

[0029] Choose SiO with n(Si / Co)=200 2 -CoO composite airgel was used as catalyst, and 0.05g, 0.15g, 0.25g and 0.35g were weighed respectively (the mass ratio of substrate styrene to catalyst was 20:1, 6.7:1, 4:1, 2.9:1 ) into four 50mL two-necked flasks, and other operating conditions are the same as in Examples 1 to 5, and the reaction results are shown in Table 2.

[0030] The influence of table 2 different catalyst dosages on epoxidation reaction

[0031]

[0032] As can be seen from Table 2, the conversion of styrene increases rapidly and slowly, and the selectivity of styrene oxide and benzaldehyde does not change much. From the consideration of cost saving, the preferred catalyst consumption is 0.25 ~ 0.35g, that is, styrene and The catalyst mass ratio is 2.9~4:1.

Embodiment example 10~12

[0033] Implementation Cases 10~12: Different n(H 2 o 2 / styrene) under the epoxidation of styrene to jointly prepare the result of styrene oxide and benzaldehyde

[0034] Choose SiO with n(Si / Co)=200 2 -CoO composite airgel as a catalyst, using n(H 2 o 2 / styrene) at 0.5, 1 and 2 of 30% hydrogen peroxide. Other operating conditions are with embodiment 1~5, and the results are shown in Table 3.

[0035] Table 3 Different n(H 2 o 2 / styrene) on the epoxidation reaction

[0036]

[0037] As can be seen in table 3, along with the increase of hydrogen peroxide consumption, styrene conversion % improves, styrene oxide selectivity % and benzaldehyde selectivity % change little, but when n(H 2 o 2 / styrene) exceeds 1, the % increase of styrene conversion rate is not obvious. In order to control the self-decomposition degree of hydrogen peroxide and reduce the danger in the production process, preferably n(H 2 o 2 / styrene) is 0.5~1:1.

[0038] Implementation Cases 13~1...

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Abstract

The invention discloses a method for jointly preparing styrene oxide and benzaldehyde by adopting SiO2-CoO composite aerogel as a catalyst, and belongs to the technical field of fine chemical preparation. The method comprises the following steps: adopting styrene as a substrate, N, N-dimethyl formamide as a reaction solvent, and 30wt% of hydrogen peroxide as an oxidizing agent for carrying out an alkene epoxidation reaction under the effect of the SiO2-CoO composite aerogel catalyst, wherein the reaction temperature is 40-80 DEG C, and the reaction time is 4-10 h; after the reaction, carrying out distillation treatment on the reaction liquid, and taking a distillation component at 180 DEG C and a distillation component at 190 DEG C respectively so as to obtain benzaldehyde and styrene oxide sequentially. The SiO2-CoO composite aerogel catalyst is simple to prepare, low in cost, capable of being used repeatedly for multiple times, convenient to operate, high in economic benefits, moderate in reaction condition, low in reaction energy consumption, low in requirements for reaction equipment, convenient to operate and environment-friendly, and the selectivity sum of styrene oxide and benzaldehyde is greater than 99%.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemical products, and in particular relates to a SiO catalyst with mild reaction conditions, simple catalyst preparation and easy separation from the reaction liquid, convenient post-processing of the product, and less environmental pollution. 2 -CoO composite airgel is a method for the joint preparation of styrene oxide and benzaldehyde with catalysts. Background technique [0002] Styrene oxide, also known as styrene oxide, is a fine chemical that can be used as an epoxy resin diluent, UV-absorber, flavor enhancer, and is also an important intermediate in organic synthesis, pharmaceutical industry, and fragrance industry body, which is mainly produced by epoxidation of styrene. [0003] Industrially, the production of styrene oxide adopts the traditional haloalcohol method and the direct oxidation method of peroxyacid. The former has many by-products and serious equipment corrosion...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/04C07D301/12C07C47/54C07C45/28
CPCB01J21/08C07C45/28C07D301/12C07D303/04C07C47/54
Inventor 张波姜剑锋邓冰心
Owner HUAWEI TEHCHNOLOGIES CO LTD
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