Method for simultaneously preparing methylallyl alcohol and cyclododecanone

A technology of methallyl alcohol and methacrolein, which is applied in the fields of oxidative preparation of carbonyl compounds, reduction preparation of oxygen-containing functional groups, organic chemistry, etc., to achieve the effects of high atom economy, high catalytic activity, and equipment cost saving

Active Publication Date: 2017-01-04
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The current production process of methallyl alcohol produces a large amount of chlorine wastewater and waste liquid. With the gradual improvement of people's requirements for environmental protection and chemical reaction atom economy, the development of low-cost, high-yield, and low-pollution production processes has become the future The inevitable trend of the development of the chemical industry, so there is an urgent need for a more green and efficient solution

Method used

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  • Method for simultaneously preparing methylallyl alcohol and cyclododecanone
  • Method for simultaneously preparing methylallyl alcohol and cyclododecanone
  • Method for simultaneously preparing methylallyl alcohol and cyclododecanone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Preparation of heteroatom-containing Y-type zeolite molecular sieve catalyst:

[0039] Add 3000g nitric acid solution (10wt%) and 600g Y-type zeolite molecular sieve into a 10L glass reactor, reflux at 90°C for 8h, filter after reflux, wash with deionized water until neutral, and dry at 120°C for 8h to obtain a Number of Y-type zeolite molecular sieves.

[0040] Dissolve tin tetrachloride and / or niobium oxalate, bismuth nitrate, and zirconium nitrate in 2% dilute nitric acid solution to obtain an active component solution, the mass concentration of the above solution is 1%, and one or more of the above solutions are used to prepare The obtained Y-type zeolite molecular sieve with a certain number of vacancies was impregnated, and then added a certain amount of auxiliary phosphoric acid, impregnated for 5 hours at 25°C, dried at 120°C for 8 hours after impregnation, and roasted at 550°C for 6 hours to obtain a finished catalyst. The specific composition is shown in Tabl...

Embodiment 2

[0044] Preparation of methallyl alcohol and cyclohexanone:

[0045] Using a 3L stainless steel reactor to synthesize methallyl alcohol and cyclohexanone, first add 1500g methacrolein, 1.5g inhibitor ZJ-701 (p-hydroxytetramethylpiperidine nitroxide free radical) and 45g catalyst, N 2 Replace the air in the system, and ensure a certain pressure, heat, stir, increase the temperature to 90 ° C, add N 2 When the pressure reached 3 bar, 214.3 g of cyclohexanol was gradually added using a parallel flow pump at a rate of 2 g / min. After the cyclohexanol was added, the reaction was continued for a total of 9 hours. After the reaction, use N 2 The materials in the system are pressed out, and the reaction kettle has its own filter head to filter to obtain a mixed solution containing cyclohexanone, methallyl alcohol and methacrolein.

[0046] The product composition was analyzed by gas chromatography. The analysis results are shown in Table 2.

[0047] Table 2 Catalytic performance of...

Embodiment 3

[0054] Different from Example 2, the reaction performance of MPV-D12 catalyst for synthesizing methallyl alcohol and cyclohexanone under different process conditions was investigated. (catalyst consumption is based on the weight of methacrolein)

[0055] Table 3 Catalyst Reaction Performance under Different Process Conditions

[0056]

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Abstract

The invention provides a method for simultaneously preparing methylallyl alcohol and cyclododecanone. According to the method, cyclohexanol is adopted as a reducing agent to supply activity H, methylacrolein is reduced in the presence of a catalyst and a polymerization inhibitor to obtain methylallyl alcohol and cyclododecanone products. The process has the characteristics of high atom economy, high product yield, mild reaction condition and no pollution.

Description

technical field [0001] The invention relates to a method for preparing methallyl alcohol and cyclohexanone, in particular to a process for reducing and preparing methallyl alcohol by using cyclohexanol as a hydrogen source and simultaneously coproducing cyclohexanone. Background technique [0002] Methallyl alcohol is an important organic intermediate used in the synthesis of perfumes, resins, etc. Using methallyl alcohol and ethylene oxide as raw materials to synthesize methallyl alcohol polyoxyethylene ether (TPEG), which is used in a new generation of high-performance concrete water reducer. It is an excellent additive in high-performance, high-strength (above C60) commercial concrete that is currently used for on-site mixing and long-distance transportation. The polycarboxylate high-efficiency superplasticizer synthesized by this product has high-efficiency particle dispersion and retention capabilities, and has many advantages such as high water-reducing rate, low ceme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/14C07C33/03C07C45/29C07C49/403
CPCC07C29/14C07C45/29C07C33/03C07C49/403
Inventor 李俊平陈海波唐敏黎源华卫琦丁建生
Owner WANHUA CHEM GRP CO LTD
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