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Preparation method of dialdehyde hemiacetal

A technology of hemiacetal and dialdehyde, which is applied in the field of preparation of dialdehyde hemiacetal, achieves the effects of simple operation, reducing the generation of by-products, and improving anti-oxidation

Active Publication Date: 2020-06-26
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are difficult problems in the existing production processes, so there is an urgent need for a more green and efficient solution

Method used

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  • Preparation method of dialdehyde hemiacetal
  • Preparation method of dialdehyde hemiacetal
  • Preparation method of dialdehyde hemiacetal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Preparation of loaded catalyst: dissolving rhodium chloride in the hydrochloric acid aqueous solution of 1mol / L to obtain concentration is the active component solution (in terms of rhodium element) of 5wt%, and palladium chloride is dissolved in the hydrochloric acid aqueous solution of 1mol / L to obtain concentration 5wt% active component solution (calculated as Pd element), then impregnate 10kg of silica carrier particles (16 mesh, specific surface area 300m 3 / g), the immersion time was 4h, and then dried at 110°C for 24h to obtain a solid; then according to the amount in Table 2, the solid was impregnated with 5wt% ammonium dihydrogen phosphate aqueous solution for 3h, then dried at 110°C for 24h, and then dried at 550 Calcined at ℃ for 4 hours to obtain a supported catalyst, which is recorded by HP number, and the preparation formula and composition of the catalyst are shown in Table 2.

[0066] Table 2 Catalyst preparation formula and composition

[0067]

[0...

Embodiment 2

[0070] use figure 1 The process flow diagram shown in the reaction.

[0071] Oxidation reaction: Set the flow rate of cyclopentene to 1.5kg / h and the flow rate of methanol to 8.5kg / h. After mixing the two, add them to a tower reactor. After all the tower reactors are full of liquid, control the temperature in the reactor to At 15°C, ozone was gradually introduced into the first, second, and third tower reactors respectively, and the total flow rate of ozone feed was 1109.6g / h, among which, the feed flow rate containing ozone in the first stage tower reactor accounted for the total flow rate 50%, the feed of the second-stage tower reactor contains 40% of the ozone flow, the feed of the three-stage tower reactor contains 10% of the ozone flow, and finally the reaction liquid flowing out from the third tower reactor passes through the fourth tower reaction The device is aged, the system pressure is controlled to 0.5MPa, the total residence time of the reaction is 4h, and the oxi...

Embodiment 3

[0074] Use different catalysts to carry out hydrogenation reaction, all the other techniques and parameters are identical with embodiment 2. The results are shown in Table 3.

[0075] Table 3 Reaction performance of different catalysts

[0076]

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Abstract

The invention relates to a preparation method of dialdehyde hemiacetal, particularly a method for preparing dialdehyde hemiacetal through two steps which are ozone oxidation and hydrogen reduction. Ozone oxidation of cycloolefin in an alcohol solvent is adopted to prepare a hemiacetal peroxide, and then hydrogen reduction is performed under the action of a catalyst to obtain the dialdehyde hemiacetal. The method for preparing the dialdehyde hemiacetal has the advantages of high reaction yield, simplicity in operation, high safety, low production cost and high industrial value.

Description

technical field [0001] The invention relates to a method for preparing dialdehyde hemiacetal, in particular to a method for preparing dialdehyde hemiacetal through ozonation reaction of cycloolefin and ozone and hydrogenation reduction. Background technique [0002] Aldehydes are highly reactive and participate in numerous reactions. Aldehydes are easily reduced to primary alcohols (-CH 2 OH). Such conversions are typically performed using catalytic hydrogenation, or direct transfer hydrogenation. It can be used to prepare special alcohols; aldehydes are easily oxidized into corresponding carboxylic acids (-COOH). The most commonly used oxidant in the industry is air or oxygen, which is one of the important methods for preparing special carboxylic acids; in addition, aldehydes can also undergo imidization reaction with amines, and then hydrogenate to prepare corresponding amines, and this route can prepare special amines class products. Since aldehyde has the above-ment...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/50C07C43/303B01J27/185
CPCC07D323/02C07C41/50C07C407/00B01J27/1856C07C43/303C07C409/20
Inventor 李俊平吴训锟张礼昌付松牟通黎源华卫琦
Owner WANHUA CHEM GRP CO LTD
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