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Preparation of methyl p-tert-butylbenzoate

A technology of methyl tert-butyl benzoate and tert-butyl benzoic acid, which is applied in the preparation of carboxylic acid esters, carboxylic acid salts, and organic compounds, and can solve the problem of affecting product purity, high equipment requirements, and dare not incinerate Disposal and other issues

Inactive Publication Date: 2018-10-16
SUQIAN COSMOS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is very efficient, it will produce a large amount of waste acid, and the post-treatment process is complicated, resulting in a large amount of waste water
[0003] Moreover, in the traditional production method, p-tert-butylbenzoic acid, the raw material for synthesizing methyl p-tert-butylbenzoate, is often oxidized with oxygen during preparation, and the oxidation kettle is always within the explosion limit range, and the attached safety protection technology Strict requirements on equipment and facilities; severe reaction heat release, harsh working conditions, high requirements on equipment; the exhaust gas is almost pure oxygen (entraining a small amount of organic gas), and dare not be incinerated, causing pollution to the environment; the by-product of benzene The amount of diformic acid is large, resulting in high consumption of raw materials and affecting the purity of the product

Method used

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  • Preparation of methyl p-tert-butylbenzoate
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Experimental program
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Embodiment approach

[0099] According to a kind of preferred embodiment of the present invention, the aftertreatment of the aqueous phase containing waste product sodium sulfate comprises the following steps:

[0100] Step a, adding inorganic alkali to the aqueous phase containing waste product sodium sulfate;

[0101] In this way, heavy metals (such as Co and Mn) therein will be precipitated and removed under alkaline conditions.

[0102] Step b, add activated carbon to carry out decolorization treatment, then filter and distill water successively to obtain solid sodium sulfate;

[0103] In this way, not only can the colored impurities in sodium sulfate be effectively removed, but also the smell of sodium sulfate can be improved to a certain extent (but activated carbon cannot remove the smell caused by sulfur-containing oligomers), greatly improving the chroma, odor.

[0104] Step c, adding the sodium sulfate solid obtained in step b into an organic solvent, reflux washing, then successively f...

Embodiment 1

[0132] (1) Transfer 500g of p-tert-butyltoluene, 0.968g of cobalt acetate, and 0.032g of manganese acetate into an oxidation kettle, raise the temperature to 125°C, and feed air at a rate of 2200mL / min to carry out the oxidation reaction. During the oxidation reaction process, control the produced water to 24-26g.

[0133] Among them, after the oxidation starts, the heat release in the oxidation process is stable. Although the reaction is stable, the temperature must be lowered, but the temperature reduction is easy to control, and strict cooling control is not required.

[0134] (2) After the oxidation reaction is completed, the material is filtered and transferred to the crystallization kettle, and the temperature is lowered and crystallized at a rate of 6°C / h, centrifuged, and p-tert-butyltoluene is washed to obtain the wet product of p-tert-butylbenzoic acid and the crystallization mother liquor , under a vacuum of 600 Pa, the temperature was raised to 105° C. at a rate of...

Embodiment 2

[0150] (1) 500g of p-tert-butyltoluene, 0.952g of cobalt acetate, and 0.048g of manganese acetate were heated up to 120°C, and air was introduced at a rate of 2000mL / min to carry out the oxidation reaction. During the oxidation reaction process, the amount of produced water is controlled to 24-26g.

[0151] Among them, after the oxidation starts, the heat release in the oxidation process is stable. Although the reaction is stable, the temperature must be lowered, but the temperature reduction is easy to control, and strict cooling control is not required.

[0152] (2) After the oxidation reaction is finished, the material is filtered and transferred to the crystallization tank, and the temperature is lowered and crystallized at a rate of 7°C / h, centrifuged, and p-tert-butyltoluene is washed to obtain the wet product of p-tert-butylbenzoic acid and the crystallization mother liquor , heating up to 110°C at a rate of 15°C / h to dry the wet product of p-tert-butylbenzoic acid to o...

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Abstract

The invention discloses preparation of methyl p-tert-butylbenzoate. The preparation of the methyl p-tert-butylbenzoate comprises the steps of oxidizing tert-butyltoluene in air by using a composite catalyst to obtain p-tert-butylbenzoic acid; and then replacing traditional concentrated sulfuric acid by using p-toluenesulfonic acid, and carrying out esterification reaction to obtain the methyl p-tert-butylbenzoate. Meanwhile, a special treatment process is used for preparation of the methyl p-tert-butylbenzoate, the yield and the purity of products are increased by repeated water carrying of methanol, meanwhile, after being treated, evaporated methanol, an extracted water phase and a catalyst are reused, the cost for raw materials is greatly reduced, and moreover, the preparation of the methyl p-tert-butylbenzoate also has important environmental protection significance.

Description

technical field [0001] The invention relates to the field of methyl p-tert-butylbenzoate, in particular to its preparation. Background technique [0002] Methyl p-tert-butylbenzoate (MBB) is an important chemical raw material for the preparation of sunscreen agent avobenzone. The current industrial preparation method is to esterify p-tert-butylbenzoic acid with methanol in the presence of a large amount of concentrated sulfuric acid to prepare MBB. However, there is a large amount of concentrated sulfuric acid used, mainly to utilize the concentrated sulfuric acid to absorb the water generated by the esterification reaction. After the esterification reaction is completed, the acid layer is removed first, washed with alkali, washed with water, and rectified to obtain the product MBB. Although this method is highly efficient, it will produce a large amount of waste acid, and the post-treatment process is complicated, resulting in a large amount of waste water. [0003] More...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/76C07C67/48
CPCC07C51/265C07C67/08C07C67/48C07C69/76C07C63/04
Inventor 马瑞孙启飞杨茂霞
Owner SUQIAN COSMOS CHEM
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