Method for co-producing 3,5-dimethylbenzoic acid and trimesic acid

A technology of dimethylbenzoic acid and trimesic acid, applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, preparation of carboxylate salts, etc. question

Active Publication Date: 2015-12-16
山东友道化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Another defect of the above method is that the product is ...

Method used

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  • Method for co-producing 3,5-dimethylbenzoic acid and trimesic acid
  • Method for co-producing 3,5-dimethylbenzoic acid and trimesic acid
  • Method for co-producing 3,5-dimethylbenzoic acid and trimesic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] The catalyst that dissolves in the fresh mesitylene that adds system is N-hydroxyl phthalimide, the metal phthalocyanine (R with general formula (IV) structure 1 = H, R 2 =H, M=Co), Co(Ac) 2· 4H 2 O and the metalloporphyrin (R 1 = R 2 = R 3 = H, M 1 = M 2 =Mn) with a total concentration of 800 ppm. When the device is in steady state operation, the flow rate of fresh mesitylene entering the primary oxidation reactor is 55.5L / h, the flow rate of the first filtrate rich in nine-carbon oxygenate intermediates is 24.9L / h, and the total flow rate is 80.4 L / h. Now the average residence time of the primary oxidation reactor in terms of liquid phase substances is 3h, and the pressurized air with an oxygen mass percentage concentration of 21% is continuously passed into the primary oxidation reactor to maintain the system reaction temperature at 120°C. The pressure is 0.5 MPa. The primary oxidation reaction solution is continuously fed into the primary separation system...

Embodiment 2

[0083] The catalyst dissolved in the fresh mesitylene added to the primary oxidation reactor is N-hydroxyphthalimide, metal phthalocyanine (R) with general formula (IV) structure 1 =OH, R 2 =H, M=Ru), cobalt naphthenate and metalloporphyrin (R 1 = R 3 = H, R 2 =OH,M 1 = M 2 =Mn), the total concentration is 10000ppm. During the steady state operation of the device, the operating process is the same as in Example 1, the operating conditions of the primary oxidation reactor are as shown in Table 1, the operating conditions of the secondary oxidation reactor are as shown in Table 2, and the operating conditions of the aging reactor are as shown in Table 3 shown. Under these operating conditions, the quality, purity, yield, yield and conversion of mesitylene are listed in Table 4 for each product obtained.

Embodiment 3

[0085] The catalyst dissolved in fresh mesitylene added to the primary oxidation reactor is CeO 2 , cobalt acetylacetonate and metallophthalocyanine (R 1 = H, R 2 =CH 3 CH 2 , M=Mn) mixture, the total concentration is 450ppm. During the steady state operation of the device, the operating process is the same as in Example 1, the operating conditions of the primary oxidation reactor are as shown in Table 1, the operating conditions of the secondary oxidation reactor are as shown in Table 2, and the operating conditions of the aging reactor are as shown in Table 3 shown. Under these operating conditions, the quality, purity, yield, yield and conversion of mesitylene are listed in Table 4 for each product obtained.

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PUM

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Abstract

The invention discloses a method for co-producing 3,5-dimethylbenzoic acid and trimesic acid. The method comprises the steps that mesitylene is taken as raw materials and processed through first-time oxidizing, first-time separating, secondary oxidizing, secondary separating, curing and third-time separating, and then the 3,5-dimethylbenzoic acid and the trimesic acid are obtained. The method has the advantages of being simple in technology, low in cost, high in yield, good in selectivity, green and environmentally friendly.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a method for co-producing 3,5-dimethylbenzoic acid and trimesic acid. Background technique [0002] 3,5-Dimethylbenzoic acid is the main intermediate in organic synthesis, mainly used in the production of tebufenozide pesticides, synthetic prostaglandins, synthetic flame retardants, plasticizers, etc., mostly using mesitylene as raw material for liquid-phase air oxidation be made of. It can be carried out in acetic acid solvent or under solvent-free conditions. The mesitylene liquid-phase air oxidation method using acetic acid as a solvent mostly uses cobalt salt as a catalyst, acetaldehyde or bromide as an initiator, and air as an oxidant. Mesitylene is oxidized to 3,5-dimethylbenzoic acid. Typical reports include the method of "Synthesis of 3,5-Dimethylbenzoic Acid by Air Catalytic Oxidation Method" disclosed in domestic Shanghai Pesticide Research Institute research ...

Claims

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Application Information

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IPC IPC(8): C07C51/265C07C51/44C07C51/43C07C63/06C07C63/307C07C63/15C07C65/30C07C51/235
CPCC07C51/235C07C51/265C07C51/43C07C51/44C07C63/06C07C63/307C07C63/15C07C65/30
Inventor 王勤波熊振华陈楚雄
Owner 山东友道化学有限公司
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