Co-production method of preparing corresponding alcohol, ester, aldehyde and acid by oxidizing p-methoxyl methylbenzene by oxygen

A technology of p-methoxytoluene and oxygen oxidation, applied in the field of daily chemical industry, can solve a large number of three wastes and other problems, and achieve the effects of reducing environmental protection pressure, easy control, and reducing manufacturing costs

Active Publication Date: 2014-07-23
SUQIAN COSMOS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Whether it is oxidation or etherification, a large amount of three wastes need to be produced, which brings pressure on environmental protection and production

Method used

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  • Co-production method of preparing corresponding alcohol, ester, aldehyde and acid by oxidizing p-methoxyl methylbenzene by oxygen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] Put 488.8Kg of acetic acid (KF<1%), 25.2Kg of cobalt acetate, 12.5Kg of manganese acetate and 122.2Kg of p-methoxytoluene into a dry stainless steel oxidation kettle. (gauge pressure) is 0.10MPa, heat preservation reaction for 6.5h, stop feeding oxygen, take samples for GC and HPLC detection, GC results are, p-methoxytoluene 51.5699%, p-methoxybenzaldehyde 25.9841%, p-methoxybenzaldehyde Benzyl alcohol 1.1660% and anisyl acetate 20.5117%, HPLC detection aldehyde-acid ratio 13.2:1.

[0066] After the oxidation reaction is finished, acetic acid KF=5.42% is recovered, and the content of acetic acid is 89.29%, which is directly used for the next batch of oxidation reaction. After recovery of acetic acid, under nitrogen protection, wash with 200Kg, 100Kg and 50Kg of clean tap water respectively, stir for 30min and then stand for stratification to obtain 399.3Kg of water phase I and 150.5Kg of oil phase I. The oil phase was taken for GC and HPLC detection. The GC results wer...

Embodiment 2

[0072]Put 488.8Kg of acetic acid (KF<1%), 25.6Kg of cobalt acetate, 19.9Kg of cerium acetate and 122.2Kg of p-methoxytoluene into a dry stainless steel oxidation kettle. After 5.0 hours of insulation reaction under normal pressure (that is, the gauge pressure is 0 MPa), stop feeding oxygen, take samples and do GC and HPLC detection, and the GC results are: p-methoxytoluene 54.4636%, p-methoxybenzaldehyde 15.2655%, Methoxybenzyl alcohol 0.6895% and anisyl acetate 27.8973%, HPLC detection aldehyde-acid ratio 39.4:1.

[0073] After the oxidation reaction is finished, acetic acid KF=5.24% is recovered, and the content of acetic acid is 88.89%, which is directly used for the next batch of oxidation reaction. After the recovery of acetic acid, under the protection of nitrogen, wash with 200Kg, 100Kg and 50Kg of clean tap water respectively, stir for 30min and then stand for stratification to obtain 407.3Kg of water phase I and 149.6Kg of oil phase I. The oil phase was taken for GC ...

Embodiment 3

[0079] Put 488.8Kg of acetic acid (KF<1%), 23.4Kg of cobalt acetate, 14.3Kg of chromium acetate and 122.2Kg of p-methoxytoluene into a dry stainless steel oxidation kettle. (gauge pressure) is 0.09MPa, heat preservation reaction for 2.5h, stop feeding oxygen, take samples for GC and HPLC detection, GC results are, p-methoxytoluene 41.1563%, p-methoxybenzaldehyde 29.5622%, p-methoxybenzaldehyde Benzyl alcohol 2.2164% and anisyl acetate 26.2614%, HPLC detection aldehyde-acid ratio 13.0:1.

[0080] After the oxidation reaction is finished, acetic acid KF=3.43% is recovered, and the content of acetic acid is 90.1%, which is directly used for the next batch of oxidation reaction. After recovery of acetic acid, under nitrogen protection, wash with 200Kg, 100Kg and 50Kg of clean tap water respectively, stir for 30min and then stand for stratification to obtain 399.3Kg of water phase I and 154.8Kg of oil phase I. The oil phase was taken for GC and HPLC detection. The GC results were ...

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Abstract

The invention relates to a co-production method for preparing corresponding alcohol, ester, aldehyde and acid by oxidizing p-methoxyl methylbenzene by oxygen. The method comprises the following steps: adding p-methoxyl methylbenzene, a catalyst I and a solvent into an oxidizing reaction kettle, and introducing oxygen to react; after oxidizing reaction, recovering the solvent and optionally selecting to apply mechanically, and then adding water to wash the catalyst I to obtain an organic phase I and an aqueous phase I; adding alkali into the organic phase I, decompressing and evaporating an organic phase II, after adding water to the bottom, adjusting the pH value by an acid, and filtering to obtain p-methoxybenzoic acid; distilling the water phase I to recover water, optionally selecting to apply mechanically, further adding the catalyst I and the solvent at the bottom, and optionally selecting to apply mechanically in oxidizing reaction; rectifying the organic phase II to obtain a product p-methoxybenzaldehyde and anisyl acetate; carrying out basic hydrolysis on anisyl acetate to obtain an anisic alcohol crude product; and rectifying to obtain an anisic alcohol pure product. The co-production method provided by the invention has the advantages of greenness and environment protection, mild reaction condition, low cost and less three waste, and is easy to industrially produce, and the obtained product is widely applied to the fields of foods, medicines and daily chemicals.

Description

technical field [0001] The invention relates to a preparation method of an organic intermediate, in particular to a co-production preparation method of p-methoxybenzyl alcohol, anisyl acetate, p-methoxybenzaldehyde and p-methoxybenzoic acid, which belongs to daily-use chemical technology field. Background technique [0002] p-Methoxybenzaldehyde (Anisic aldehyde), is a colorless to pale yellow liquid at room temperature, with a hawthorn-like smell. Density 1.123g / cm 3 (20°C). Melting point 0°C. The boiling point is 249.5°C. The refractive index is 1.5731. Insoluble in water, easily soluble in ethanol, ether, acetone, chloroform. With water vapor can be volatile. It exists in fennel oil, cumin oil, dill oil, acacia flower, and vanilla extract in nature, and is obtained by oxidation, separation and extraction. It is used as a spice to prepare flower-flavored essence, used in food, cosmetics, soap, etc. In medicine, it is used as an intermediate of antihistamines, such...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/23C07C41/26C07C47/575C07C45/36C07C65/21C07C51/265C07C69/16C07C67/39
CPCC07C41/26C07C45/36C07C51/265C07C67/08C07C65/21C07C47/575C07C69/16C07C43/23
Inventor 刘启发宋小明王荣张彬彬高元
Owner SUQIAN COSMOS CHEM
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