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Method for producing meta benzene tricarbonic acid through sequential oxidation by using intermittent multiple cascaded Bubbling oxidation towers

A technology of trimellitic acid and oxidation tower, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc. It can solve the problems of easy leakage and damage of moving sealing parts, easy blockage of crystallizer inlet, unfavorable crystal growth, etc. problems, achieve stable and reliable operation, improve energy conversion efficiency, and stabilize product quality

Active Publication Date: 2007-02-21
NANTONG BAICHUAN NEW MATERIAL CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] 1. The reaction time is long, the reaction is incomplete, there are many by-products, the quality is unstable, and the product yield is low. At present, the molar yield of trimellitic acid process products produced by batch method is 65-80%.
[0006] 2. During the intermittent production process, the reactor needs to be repeatedly boosted and lowered, and the temperature raised and lowered. The equipment is prone to fatigue and the service life is shortened.
[0007] 3. Oxidation step may enter the explosion hazard zone every time the temperature is raised and the pressure is raised. There is a danger of explosion if there is a slight carelessness, and the production safety is very low.
The equipment investment of the pressurized stirring type clean kettle is expensive, and there is a problem that the moving sealing parts are easy to leak and damage
Continuous operation cannot change the temperature, which is not conducive to crystal growth, and the crystallization effect is poor. The mother liquor with incomplete crystallization must be recycled to achieve the purpose of crystallization and separation.
Moreover, the multi-pot continuous crystallization has the problem that the inlets of each crystallizer are easy to block when feeding
Single tank (kettle) continuous operation, because the temperature cannot be changed, the crystallization effect is even worse

Method used

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  • Method for producing meta benzene tricarbonic acid through sequential oxidation by using intermittent multiple cascaded Bubbling oxidation towers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] a) 1000Kg unimitylene is sent into 1# batching still 7 through metering tank 6 and 5 respectively from solvent tank 3 with delivery pump 2 and solvent pump 4 from raw material tank 1,4000Kg acetic acid solvent 4000Kg, weighs cobalt acetate, Put 4.5Kg each of manganese acetate and tetrabromoethane into 1# batching kettle 7, heat to 80°C, and stir fully at the same time until the catalyst is completely dissolved;

[0034] b) Turn on soft water pump 35 and add soft water to 1# condenser 12 and 2# oxidation condenser 15 to keep the soft water level at 60% to 80%; 3 / h is sent into 1# oxidation tower 13, stops charging when reaching setting liquid level 50%~60%, opens circulation pump 14 and circulates material in 1# oxidation tower 13, and the material in the tower is heated, simultaneously to Continuously feed compressed air 11 into the tower to gradually increase the temperature and pressure to initiate the oxidation reaction. After the initiation is successful, the tempe...

Embodiment 2

[0042] a) 1500Kg unimitylene from raw material tank 1, 7500Kg acetic acid solvent from solvent tank 3 with delivery pump 2 and solvent pump 4 are sent into 1# batching kettle 7 through metering tank 6 and 5 respectively, weigh cobalt acetate 4.5 respectively kg, manganese acetate 2.5kg, tetrabromoethane 3.8Kg drop into 1# batching kettle 7, measure acetic acid 300kg through measuring tank 5, weigh respectively cobalt acetate 2.5kg, manganese acetate 4.5kg, tetrabromoethane 3.8Kg drop into 2# The batching kettle 9 is heated to 80°C respectively, and at the same time, it is fully stirred until the catalyst is completely dissolved;

[0043] b) Turn on soft water pump 35 and add soft water to 1# condenser 12 and 2# oxidation condenser 15 to keep the soft water level at 60% to 80%; 3 / h is sent into 1# oxidation tower 13, stops charging when reaching setting liquid level 50%~60%, opens circulation pump 14 and circulates material in 1# oxidation tower 13, and the material in the tow...

Embodiment 3

[0050] a) 1000Kg unimitylene is sent into 1# batching kettle 7 through metering tank 6 and 5 from raw material tank 1, 6000Kg acetic acid solvent from solvent tank 3 with delivery pump 2 and solvent pump 4 respectively, and weighs cobalt acetate 4.0 respectively kg, manganese acetate 1.1kg, tetrabromoethane 2.4Kg drop into 1# batching kettle 7, measure acetic acid 300kg through measuring tank 5, weigh respectively cobalt acetate 1.1kg, manganese acetate 4.0kg, tetrabromoethane 3.0Kg drop into 2# The batching kettle 9 is heated to 80°C respectively, and at the same time, it is fully stirred until the catalyst is completely dissolved;

[0051] b) Turn on soft water pump 35 and add soft water to 1# condenser 12 and 2# oxidation condenser 15 to keep the soft water level at 60% to 80%; 3 / h is sent into 1# oxidation tower 13, stops charging when reaching setting liquid level 50%~60%, opens circulation pump 14 and circulates material in 1# oxidation tower 13, and the material in the...

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Abstract

This invention relates to a method for preparing trimellitic acid with series intermediate bubble oxidization columns by continuous oxidation. The method comprises: (1) mixing 1,2,4-trimethylbenzene with solvent and catalyst in a kettle, heating for mixing, and sending to a series of three oxidization columns for reaction; (2) introducing the reaction products into a crystallization kettle, crystallizing to obtain mixed slurry of trimellitic acid crystal, acetic acid and water, sending to a centrifugation separator for separation, and sending the w trimellitic acid granules to the anhydridization process; (3) sending the mixture of acetic acid and water to a concentration column, and recovering acetic acid for recycling; (4) recovering trimellitic acid from the concentration column bottom product in a flash evaporation column. The series oxidization columns have such advantages as low investment, no leakage, no blockage at the inlet / outlet, continuous operation, high productivity, high yield, low raw material consumption and low energy consumption.

Description

technical field [0001] The invention relates to a method for producing trimellitic acid by continuous oxidation in series with multiple towers of intermittent bubbling oxidation towers. It belongs to the field of organic chemical technology. Background technique [0002] Trimellitic acid is an important raw material for the production of trimellitic anhydride. Trimellitic anhydride is an important organic chemical raw material for modern new materials. It has high reactivity and can produce a series of fine chemicals with high added value. It is mainly used in engineering plastics, high-quality plasticizers, heat-resistant insulating varnishes, advanced coatings, etc. industry. Because the resin material made of it has excellent electrical insulation, high temperature resistance and mechanical properties, it is also widely used in industrial fields such as electromechanical, electronic and aerospace. [0003] At present, the method for producing trimellitic acid mainly ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/307C07C51/265
Inventor 郑铁江高峰
Owner NANTONG BAICHUAN NEW MATERIAL CO LTD
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