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Treatment method of waste residue in the production of high content rubber anti-aging agent tmq

A treatment method and technology of anti-aging agent, applied in the direction of organic chemistry, etc., can solve the problems of polluting the environment and the inability to treat waste residues, achieving the effect of environmental protection and significant economic benefits, and saving the cost of waste residue treatment

Active Publication Date: 2017-12-05
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Each ton of high-content TMQ produces about 80kg of waste residue, a large amount of waste residue cannot be treated and pollutes the environment

Method used

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  • Treatment method of waste residue in the production of high content rubber anti-aging agent tmq
  • Treatment method of waste residue in the production of high content rubber anti-aging agent tmq

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Condensation: Mix 100kg of residue, 10kg of aniline, 200kg of acetone, and 10kg of monomer in a reactor, and heat up to polycondense; the reaction temperature is 50°C, and the reaction is 3h; the acetone is distilled and recovered after the reaction;

[0022] (2) Neutralization: Prepare a 5% sodium hydroxide solution, add it dropwise to the condensation kettle, and at the same time add silicone defoamer S909 until there is no obvious foam; stop adding when the pH value reaches 6, and let it stand for 30 minutes Separate the aqueous layer;

[0023] (3) The oil phase enters the monomer still, and the distillation temperature is 200°C; when there is no reflux in the sight glass, the distillation is stopped, and the finished product is cooled and granulated; the softening point is 92°C, and the effective content is 43%. Agent RD national standard.

Embodiment 2

[0025] (1) Condensation: Mix 100kg of residue, 10kg of aniline, 300kg of acetone, and 10kg of monomer in a reaction kettle, and heat up for polycondensation. The reaction temperature was 75°C, and the reaction was carried out for 2 hours; the acetone was distilled and recovered after the reaction;

[0026] (2) Neutralization: prepare potassium hydroxide solution with a mass concentration of 7%, drop it into the condensation kettle, and add polyether defoamer GP330 dropwise until there is no obvious foam; stop dropping when the pH value reaches 7, and let it stand for 30 minutes Afterwards, the aqueous layer was separated;

[0027] (3) The oil phase enters the monomer still, and the distillation temperature is 230°C. When there is no reflux in the sight glass, stop the distillation, cool down and granulate to obtain the finished product; the softening point is 88°C, the effective content is 43%, and all indicators meet the national standard of ordinary anti-aging agent RD.

Embodiment 3

[0029] (1) Condensation: Mix 100kg of residue, 50kg of aniline, 500kg of acetone, and 10kg of monomer in a reactor, and heat up for polycondensation; the reaction temperature is 100°C, and the reaction is 1 hour; the acetone is distilled and recovered after the reaction

[0030] (2) Neutralization: configure a 10% sodium hydroxide solution with a mass concentration, add it dropwise to the condensation kettle, and add the high-carbon alcohol defoamer 2,6-dimethyl-4-heptanol dropwise until there is no obvious foam; when the pH Stop dripping when the value reaches 7, and the water layer is separated after standing for 30min;

[0031] (3) The oil phase enters the monomer still, and the distillation temperature is 250°C. When there is no reflux in the sight glass, stop the distillation, cool down and granulate to obtain the finished product; the softening point is 91°C, the effective content is 45%, and all indicators meet the national standard of ordinary anti-aging agent RD.

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Abstract

The present invention relates to a method for processing waste residues in high content rubber antioxidant TMQ production process, the method is as follows: the waste residues are mixed with quantitative aniline, quantitative acetone and a quantitative monomer for dilution; reaction is performed at certain temperature for certain time; then a dilute alkaline solution is added dropwise, and a defoamer is added until no obvious bubble is in the solution; when the PH value reaches 6-7, the dropwise addition is stopped, and water is separated after standing; oil phase is transferred into a distillation kettle for monomer distillation for recovery of the monomer; the distillation is stopped when no reflux is observed by sight glass; after cooling, granulation is performed, softening point and active ingredient content are detected, and general antioxidant TMQ index requirements can be met. According to the method, by treatment of the waste residues in the high content rubber antioxidant TMQ production process, general antioxidant TMQ product indexes can be reached, hazardous solid waste production can be effectively reduced, and general antioxidant TMQ production cost can be reduced.

Description

technical field [0001] The invention belongs to a method for treating waste of rubber additives, in particular to a method for treating waste residue in the production of high-content rubber anti-aging agent TMQ. Background technique [0002] Rubber Antiaging Agent TMQ is an oligomer of 2,2,4-trimethyl-1,2-dihydroquinoline with a degree of polymerization of 2-4. It is a ketone-amine antiaging agent and is light yellow to amber in color. Powder or flake, is a general-purpose amine antioxidant with excellent heat and oxygen aging resistance in the rubber industry. It is widely used in the production of radial tires and other rubbers due to its low toxicity and good compatibility in rubber. It is one of the rubber antioxidant products with the largest demand in domestic and foreign markets. Currently commercially available products are divided into ordinary anti-aging agent TMQ and high-content anti-aging agent TMQ. Ordinary anti-aging agent TMQ two, three, tetramer content r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/3437C07D215/06
CPCC07D215/06C08K5/3437
Inventor 安静李家元李润才
Owner KEMAI CHEM