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Synthesis process of methylacrolein

A technology for the synthesis of methacrolein, which is applied in the direction of carbon-based compound preparation, organic compound preparation, organic compound/hydride/coordination complex catalyst, etc., and can solve the difficulty of industrial production and the yield of methacrolein It is difficult to improve the difficulty, yield and high selectivity are difficult to balance, to achieve the effect of improving selectivity and yield, saving costs, and avoiding complex reaction conditions

Pending Publication Date: 2022-05-24
郑州中科新兴产业技术研究院 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Aiming at the technical problems that the yield of methacrolein is difficult to increase, the yield and high selectivity are difficult to balance, and the industrial production is difficult, the present invention proposes a synthesis process of methacrolein to achieve the preparation of methacrolein with high selectivity and high yield, can realize the purpose of industrialized production

Method used

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  • Synthesis process of methylacrolein
  • Synthesis process of methylacrolein
  • Synthesis process of methylacrolein

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A synthesis technique of methacrolein, the specific operation steps of the synthesis technique are: firstly add 17.4g of morpholine in the reaction flask, dropwise add 11.4g of glacial acetic acid under room temperature conditions (the mol ratio of glacial acetic acid and morpholine is 0.95 g) ), add deionized water to the reaction system before the dropwise addition; after the dropwise addition, stir evenly to obtain a morpholine acetate solution, then heat up to 40 ° C, continue to stir, and then add the polymerization inhibitor nitroxyl piperidine Alcohol 1.7g, start to slowly drip the mixed solution of formaldehyde and propionaldehyde, in the mixed solution, formaldehyde 31.5g, propionaldehyde 58.0g (the mol ratio of formaldehyde and propionaldehyde is 1.05, the mol ratio of morpholine acetate solution and propionaldehyde is 0.2), after the dropwise addition, continue to react for a certain period of time, after the completion of the reaction, the reaction solution i...

Embodiment 2

[0027] The synthesis technique of methacrolein, the concrete operation steps of its synthesis technique and the difference of embodiment 1 are the mol ratios 0.8, 0.9, 1.0, 1.1, 1.2 of formaldehyde and propionaldehyde. The aldehydes are numbered I, II, III, IV, and V. The products obtained after the reaction were sampled and detected by GC, respectively, to obtain the conversion rate of propionaldehyde and the yield and selectivity of methacrolein. The experimental data are shown in Table 1.

[0028] Table 1 embodiment 2 methacrolein product detection result

[0029]

[0030] As can be seen from the above table, the conversion rates of the propionaldehyde groups III and IV are all above 99%, and the yield and selectivity of methacrolein are also above 90%. Therefore, it can be seen that the synthesis of the technical solution of the present application The process can take into account high yield and high selectivity at the same time, and compared with the existing methacro...

Embodiment 3

[0032] The synthesis technique of methacrolein, wherein the mol ratio of formaldehyde and propionaldehyde is 1.0, the mol ratio of acetic acid and morpholine is 0.7, 0.9, 1.1, 1.3, 1.5, and the above-mentioned different mol ratios of acetic acid and morpholine are respectively synthesized The number of methacrolein is i, ii, iii, iv, ⅴ;

[0033] Other steps are the same as in Example 1.

[0034] The product obtained after the reaction was sampled and detected by GC to obtain the conversion rate of propionaldehyde and the yield and selectivity of methacrolein. The experimental data are shown in Table 2.

[0035] The detection result of table 2 embodiment 3 methacrolein product

[0036]

[0037] It can be seen from the experimental data in the above table that with the increase of the ratio of glacial acetic acid and morpholine, the conversion rate of propionaldehyde and the yield of MAL showed a trend of first increasing and then decreasing. Comparing ⅰ-ⅴ, it can be seen t...

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Abstract

The invention provides a synthesis process of methylacrolein, which is used for solving the problems that the yield of methylacrolein is difficult to increase, and the yield and high selectivity are difficult to consider at the same time, and a morpholine acetate solution catalyst system is prepared by mixing morpholine and glacial acetic acid. Methacrolein is prepared by catalyzing a mixed solution of formaldehyde and propionaldehyde with a morpholine acetate solution. Formaldehyde and propionaldehyde are subjected to a Mannich reaction process to generate methylacrolein, the addition of acetic acid can effectively promote the transfer rate of protons in the Mannich decomposition process, the addition of a polymerization inhibitor effectively inhibits side reactions, and the reaction yield and selectivity are improved. According to the method, the morpholine acetate solution is used as the catalyst, so that the selectivity and the yield of the methylacrolein are improved; meanwhile, compared with existing condensation reaction conditions, the corrosion is small, the reaction is carried out under the conditions of normal pressure and 30-60 DEG C, the reaction conditions are mild and controllable, and good stability is achieved.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a synthesis process of methacrolein. Background technique [0002] Methacrolein (MAL), an important organic chemical intermediate, has a wide range of uses and can be used to synthesize methacrylic acid, methallyl alcohol, methyl methacrylate, isopropyl methacrylate and thermoplastics Monomers and other chemical products. Methacrolein, its appearance is light yellow liquid with strong pungent odor, boiling point 68℃, slightly soluble in water, easily soluble in ethanol and ether, moderately toxic. [0003] Its traditional acetone cyanohydrin method (ACH) for synthesizing methacrolein has been eliminated due to its heavy pollution and low atomic utilization rate. At present, there are mainly the following relatively mature process routes: isobutylene / tert-butanol catalytic oxidation method, isobutylene Butane direct oxidation method, formaldehyde and propionaldehyde condensation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/74C07C47/22B01J31/04B01J31/02
CPCC07C45/74B01J31/04B01J31/0235B01J31/0271C07C47/22Y02P20/584
Inventor 李杰孙威赵秋曹莎莎常炜张国梁李春山
Owner 郑州中科新兴产业技术研究院
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