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Comprehensive utilization method for aromatic carboxylic acid residues

A technology of aromatic carboxylic acid and residue, which is applied in the field of utilization of aromatic carboxylic acid residue, can solve the problems of incomplete utilization of residue, waste of chemical raw materials and energy, environmental pollution, etc., and achieves obvious toughening effect, low cost, and improved dispersion effect of effect

Inactive Publication Date: 2013-10-23
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, TA residues are mainly treated by incineration, which not only causes environmental pollution, but also causes waste of chemical raw materials and energy such as benzoic acid and terephthalic acid in the residues. Therefore, the comprehensive utilization of TA residues has always been an important issue in the chemical industry. Problems to be solved in the field
Patent CN1278272A discloses a method of incinerating TA residue as boiler fuel; CN1611482A discloses a method of recovering terephthalic acid and isophthalic acid in the residue by methyl esterification, rectification, recrystallization and transesterification. and the method of benzoic acid; CN1253942A discloses a method of reclaiming benzoic acid from TA residue by distillation under reduced pressure; CN1078738A, CN101054450A and CN1031540A disclose respectively taking TA residue as raw material by steps such as esterification and separation to prepare plastic stabilizer, The methods of polyurethane coating and polyester resin, these methods provide a new way for the comprehensive utilization of TA residues, these methods are either complicated in process, or cannot realize the complete utilization of residues

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] The residue after drying the raffinate used in the embodiment of the present invention mainly contains benzoic acid, phthalic acid, isophthalic acid, terephthalic acid, p-toluic acid, etc., wherein the content of each substance is: benzoic acid is 25 ~ 30%, the content of benzenedicarboxylic acid is 45-75%, and the total acidity is 43.3969gNaOH / 100g.

[0024] (1) Accurately weigh 0.5000g of TA residue, dissolve it in hot water (temperature 50°C), slowly titrate with standard NaOH solution, and calculate the total acidity, which is used to calculate the amount of basic compound required for salt formation. Preparation of carboxylate;

[0025] (2) Weigh 100g of TA residue, add it to 50g of 50°C hot water, add 111g of calcium bicarbonate to it under stirring, and fully react and neutralize;

[0026] (3) filter, the filtrate is evaporated or naturally volatilized to dryness, and the solid is crushed to 600 mesh to obtain the residue calcium salt;

[0027] (4) Get residue ...

Embodiment 2

[0031] With the TA residue described in Example 1,

[0032] (1) Accurately weigh 0.5000g of TA residue, dissolve it in hot water, slowly titrate it with standard NaOH solution, and calculate the total acidity, which is used to calculate the amount of basic compound required for salt formation and for the preparation of carboxylate ;

[0033] (2) Weigh 100.0g of TA residue, add it to 50g of hot water, add 61.3g of CaO to it under stirring, and fully react and neutralize;

[0034] (3) filter, the filtrate is evaporated or naturally volatilized to dryness, and the solid is crushed to 800 mesh to obtain the residue calcium salt;

[0035] (4) Get residue calcium salt 50g, polypropylene (T30S) 250g, white oil 3g, stir evenly, add in the extruder, extrude granulation, obtain β-nucleating agent masterbatch;

[0036] (5) In the production of PP, 0.4% by mass β-nucleating agent masterbatch can be added to obtain toughened polypropylene.

[0037] The impact strength of PP without nucl...

Embodiment 3

[0039] With the TA residue described in Example 1,

[0040] (1) Accurately weigh 0.5000g of TA residue, dissolve it in hot water, slowly titrate it with standard NaOH solution, and calculate the total acidity, which is used to calculate the amount of basic compound required for salt formation and for the preparation of carboxylate ;

[0041] (2) Weigh 100g of TA residue, add it to 50g of hot water, add 61.5g of Mg(OH) to it under stirring 2 , full response;

[0042] (3) filter, the filtrate is evaporated or naturally volatilized to dryness, and the solid is crushed to 600 mesh to obtain the residue magnesium salt;

[0043] (4) Get residue magnesium salt 50g, polypropylene (T30S) 250g, white oil 3g, stir evenly, add in the extruder, extrude granulation, obtain β-nucleating agent masterbatch;

[0044] (5) In the production of PP, a β-nucleating agent masterbatch with a mass percentage of 0.6% can be added to obtain toughened polypropylene.

[0045] The impact strength of PP ...

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Abstract

The invention relates to a comprehensive utilization method for aromatic carboxylic acid residues. An appropriate amount of alkali compound is added into romatic carboxylic acid raffinate or the aromatic carboxylic acid residues to perform reaction till the raffinate or the residues is / are neutral, and moisture in a reaction solution is removed to obtain residue metal salt. The residue metal salt and polypropylene powder or granules are mixed according to the weight ratio of 1:5-20, an appropriate amount of white oil is added into a mixture, extrusion and granulation are performed to obtain beta-nucleating agent master-batches, the beta-nucleating agent master-batches are added during the polypropylene processing to obtain toughened polypropylene. By means of the comprehensive utilization method, the residues are directly used or neutralized and converted into the metal salt. The method is simple and convenient and low in cost, 100% of comprehensive utilization of tantalum residues is achieved, no secondary pollution is caused, and energy consumption is very low.

Description

technical field [0001] The invention relates to a method for utilizing aromatic carboxylic acid residues, in particular to a toughening method for converting TA residues into metal salts and using the salts as beta-nucleating agents for polypropylene. Background technique [0002] The process of producing polyester resin will produce a large amount of aromatic carboxylic acid residues (TA residues), whose main components include benzoic acid, terephthalic acid, isophthalic acid, p-toluic acid, etc. The components are complex and difficult to recycle. A factory with an annual output of 1 million tons of PTA will have a residue volume of 5,000 tons a year. At present, TA residues are mainly treated by incineration, which not only causes environmental pollution, but also causes waste of chemical raw materials and energy such as benzoic acid and terephthalic acid in the residues. Therefore, the comprehensive utilization of TA residues has always been an important issue in the ch...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08L23/12C08K5/098C08J3/22
Inventor 周传健关瑞芳
Owner SHANDONG UNIV