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Process for producing isophthalic acid

A technology of isophthalic acid and m-xylene, which is applied in the direction of carboxylate preparation, organic compound preparation, organic compound/hydride/coordination complex catalyst, etc., can solve the problem of long residence time, increased device construction cost, Reduce the combustion reaction rate, minimize environmental pollution, and reduce equipment corrosion due to problems such as rising production costs

Inactive Publication Date: 2013-01-30
EAST CHINA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0011] Acetic acid and m-xylene are oxidized to generate carbon dioxide and carbon monoxide, resulting in increased loss of acetic acid and reduced product yield, which not only increases production costs but also pollutes the environment
The reason is that the Co-Mn-Br catalytic system adopted is a homogeneous catalytic system, which is uniformly mixed with the solvent acetic acid and the product isophthalic acid of the reaction in the reactor, and the CSTR reactor makes the reaction product stay in the reactor. If the time is too long, it will not only increase the combustion consumption of isophthalic acid, but also increase the emission of greenhouse gas carbon dioxide, so it is unreasonable to use CSTR reactor to produce isophthalic acid
[0012] At the same time, due to the strong corrosiveness of bromide ions, expensive corrosion-resistant materials must be used, which increases the cost of device construction; the generated methyl bromide gas will destroy the ozone layer and cause environmental pollution.

Method used

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  • Process for producing isophthalic acid
  • Process for producing isophthalic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The coconut shell gac of 15g is soaked in the phosphomolybdovanadic acid (H 6 PMo 9 V 3 O 40 ·5H 2 O) in an aqueous solution, heated to reflux for 6 hours, filtered, washed with hot water until neutral, drained, dried at 110°C for 4 hours, then activated at 350°C for 12 hours under the protection of nitrogen to obtain a loading capacity of 10% (weight) of H 6 PMo 9 V 3 O 40 / C Catalyst.

[0034] The experiment was carried out in a stirred reactor with a volume of 1000ml, adding 400ml of glacial acetic acid, 50g of water, 25g of m-xylene, 5g of the previously prepared 40-60 mesh activated carbon supported heteropolyacid catalyst, the reaction temperature was 210°C, and the pressure was 13MPa. The flow rate of air is 1 L / min, the reaction is 30 minutes, the conversion rate of m-xylene is 100%, and the yield of isophthalic acid reaches 95%.

Embodiment 2

[0036] The preparation method of activated carbon-supported heteropolyacid catalyst is as in Example 1.

[0037] The experiment was carried out in a fixed-bed reactor with a height of 80 cm and an inner diameter of 2 cm, which contained 10-20 meshes of activated carbon-loaded heteropolyacid catalysts. The gas-liquid two-phase flowed through the reactor from bottom to top, and the flow rate of the liquid was 10ml / min. The flow rate of air 500ml / min, in the liquid feed, m-xylene 15% (weight), water 20% (weight), all the other are acetic acid, 210 ℃ of reaction temperatures, pressure 13MPa, m-xylene conversion rate 50%, m-xylene Diformic acid yield reached 49%.

Embodiment 3

[0039] 15g of coal-based activated carbon was immersed in 20% phosphotungstic acid (H 3 PW 12 O 40 ) in an aqueous solution, heated to reflux for 4 hours, filtered, washed with hot water until neutral, drained, dried at 110°C for 5 hours, and activated at 300°C for 10 hours under the protection of nitrogen to obtain a loading capacity of 15 % (weight) of H 3 PW 12 O 40 / C catalyst.

[0040] Experimental research was carried out under the same conditions as in Example 1. After 35 minutes of reaction, the conversion rate of m-xylene was 100%, and the yield of isophthalic acid reached 94%.

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Abstract

The invention relates to a method for producing isophthalic acid by using m-xylene. In a reactor, under the atmosphere of 6 to 20 and at the temperature of between 150 and 300 DEG C, a gas-liquid-solid three-phase reaction system is formed by the m-xylene serving as a raw material, air serving as an oxidant, acetic acid serving as solvent and active carbon loaded with 5 to 60 weight percent of heteropolyacid serving as a solid catalyst to oxide the m-xylene into the isophthalic acid. The method can reduce the combustion reaction rate of the acetic acid and the m-xylene, reduce the losses of the acetic acid and the m-xylene, avoid using bromine, reduce equipment corrosion, reduce pollution to environment, and realize green production of the isophthalic acid.

Description

technical field [0001] The invention relates to a process for producing isophthalic acid. Background technique [0002] Isophthalic acid (IPA) is also known as 1,3-phthalic acid or iso-titanic acid, 1,3-benzenedicarboxylic acid, isophthalic acid, or m-phthalic acid. Molecular formula is C 8 h 6 O 4 , with a molecular weight of 166.13, colorless needle-like crystals, with strong heat resistance, hydrolysis resistance and chemical resistance. IPA can undergo reactions such as salt formation, dehydration, hydrogenation, and halogenation. It is mainly used in the production of polyester, coatings, special fibers, hot-melt adhesives, printing inks, polyester fiber dyeing modifiers, and resin plasticizers. It is a promising intermediate material. [0003] At present, the consumption of isophthalic acid in the world is mainly reflected in several aspects such as unsaturated polyester resin, polyester and alkyd resin (mainly used as surface coating), ink, plasticizer and interm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C63/24C07C51/265B01J31/04
Inventor 龙湘犁吕海锋刘念袁渭康
Owner EAST CHINA UNIV OF SCI & TECH
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