Anti-aging agent TMQ and preparation method thereof

A technology of anti-aging agent and rubber anti-aging agent, applied in the direction of organic chemistry, can solve the problems of high price, large amount of three wastes, and corrosion of equipment, and achieve the effects of low catalyst consumption, high effective body content, and low production cost

Inactive Publication Date: 2018-05-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that after the catalyst p-toluenesulfonic acid and zinc chloride are consumed, they cannot be regenerated and recycled, resulting in more waste liquid and corrosion of equipment.
CN102153511 discloses a method for preparing 2,2,4-trimethyl-1,2-dihydroquinoline polymer (anti-ageing agent TMQ), which uses aniline and acetone to continuously enter the reaction process equipped with a solid acid catalyst Tower, the reactants are then condensed, this method is easy to operate, the amount of waste water is small, but the s

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Batch reaction mode: put 250g of aniline and 5g of diisopropyl titanate into 1000m1 with agitator, thermometer and discharge pipeline (connected to a fractionation tower, so that acetone and the water produced by the reaction enter the fractionation tower) in a four-neck flask. Under normal pressure, 1500 g of acetone was continuously fed by a metering pump, the feeding reaction time was 6 hours, and the reaction temperature was controlled at 130° C. to prepare the antioxidant TMQ feed liquid. The water produced during the reaction and the excess acetone pass through the fractionation tower, the acetone can be recovered at the same time, and the water produced by the reaction can be separated. The one-way conversion rate of aniline in the reaction can reach 80%. Finally, neutralize the anti-aging agent TMQ feed liquid with 3g of liquid alkali, static layering, the lower layer of wastewater into the wastewater treatment system, and the upper layer of feed liquid through ...

Embodiment 2

[0025] Continuous tower reaction mode: control the feed weight ratio of tetraisopropyl titanate, aniline and acetone to 1:450:1100. Aniline is continuously fed from the top of the tower, and after the acetone is vaporized, it is fed from the gas phase at the bottom of the tower, and the continuous reaction is carried out in the tower. The acetone and the water produced by the reaction are passed through the fractionating tower connected to the top of the reaction tower to reclaim the acetone and the water produced by the separation reaction, and the polycondensation liquid of the antioxidant TMQ generated by the reaction continuously flows into the receiving tank at the bottom of the tower, wherein the conversion rate of aniline is 80.4 %. Finally, add 5% sodium hydroxide 3g to the anti-aging agent TMQ polycondensation solution, neutralize to weak alkalinity, stand and separate, and the upper oil phase is subjected to vacuum distillation at -0.098MPa, and unreacted aniline is ...

Embodiment 3

[0027]Batch reaction method: put 250g of aniline and 2g of tetra-n-butyl titanate catalyst into 1000m1 at one time, with agitator, thermometer and discharge pipeline (connected to a fractionation tower, so that acetone and the water produced by the reaction enter the fractionation tower ) in a four-necked flask, 1600g of acetone was fed in the form of a metering pump continuous feed, and the feed reaction time was 4 hours. Under normal pressure, the reaction temperature is controlled at 140 °C, and the reaction water and excess acetone pass through the fractionation tower to simultaneously recover acetone and separate the reaction water. The kettle liquid is TMQ polycondensation liquid, and the one-pass conversion rate of aniline in the reaction can reach 81.5%. Add 1g of 25% sodium bicarbonate to neutralize to weak alkalinity, let stand to separate and separate, and the upper oil phase is subjected to -0.098MPa vacuum, and the unreacted aniline and TMQ monomers are recovered b...

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Abstract

The invention provides an anti-aging agent TMQ and a preparation method thereof. The preparation method comprises preparing the anti-aging agent TMQ for rubber from aniline and acetone (or isopropylideneacetone) as raw materials in the presence of a catalyst through a one-step method. The catalyst comprises a titanate catalyst. The anti-aging agent TMQ for rubber is prepared through the preparation method. The preparation method utilizes a batch or continuous production process. A single-pass conversion of aniline is 80% or more. The content of the product TMQ effective bodies (such as dimer,trimer and tetramer) is 65% to 75%. Compared with the prior art, the preparation method utilizing the titanate catalyst to prepare the rubber anti-aging agent TMQ is an eco-friendly method having theadvantages of simple processes, low catalyst consumption, low cost and high effective body content.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, relates to a preparation method of anti-aging agent TMQ, and is a green and environment-friendly preparation process. Background technique [0002] Antiaging agent TMQ is the two, three, and tetrapolymers of 2,2,4-trimethyl-1,2-dihydroquinoline, also known as antiaging agent RD. It is a ketamine antiaging agent, which is light yellow to Xubo color granules or flakes are mainly used as rubber anti-aging agent, and it is one of the most demanded rubber anti-aging agent products in the domestic and foreign markets. [0003] The main raw materials for the synthesis of anti-aging agent TMQ are aniline and acetone (or its derivatives), and the process can be roughly divided into "one-step method" or "two-step method". The "one-step method" is: condensation and polymerization of aniline and acetone under the action of a catalyst to directly obtain di-, tri-, and tetra-polymers containing 2,2,4-t...

Claims

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Application Information

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IPC IPC(8): C07D215/06C08K5/3437
CPCC07D215/06C08K5/3437
Inventor 刘建韦志强
Owner CHINA PETROLEUM & CHEM CORP
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