Continuous production method for vulcanization accelerator DPG

A vulcanization accelerator and production method technology, applied in the field of rubber accelerators, can solve problems such as increased process risk, high safety risk, and large amount of ammonia water feeding, and achieve the effects of improving the intrinsic safety of the process, shortening the reaction time, and reducing the risk of explosion

Active Publication Date: 2018-09-28
KEMAI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process uses ethanol instead of water as the solvent and diluent for the reaction, and uses ammonia instead of ammonia water as the reaction raw material to avoid the generation of waste water, but in the overall reaction process, oxygen and ammonia will be fed into the reactor at the same time according to a fixed ratio. Although the solvent ethanol can dissolve part of the ammonia, but because the solubility of ammonia in ethanol is not high, there is obviously a mixed atmosphere of ammonia and oxygen within the explosion limit range in the system, which is very prone to explosion, and the process is inherently safe. Very large and does not have industrial value
Moreover, this process also requires high-temperature ethanol solution to filter and separate the product ammonium sulfate (that is, the filter cake obtained from the high-temperature filtration of the primary product), which further increases the safety risk of the overall process and makes it unsuitable for industrialization.
[0007] In addition, the current synthesis process of the accelerator DPG mainly uses tank reactors for intermittent operation, and the factors between batches are greatly affected by personnel operations, and the product quality is prone to instability.
At the same time, during the kettle oxidation process, the amount of ammonia water is large, and the unreacted ammonia and oxygen are likely to form explosive mixtures, which increases the process risk.
At the same time, the manufacturing cost of the pressure reactor is relatively high, and it is prone to problems in long-term operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] A continuous production method of vulcanization accelerator DPG, comprising the steps of:

[0048] (1) 400g diphenylthiourea, 0.5g catalyzer copper acetate and 372mL concentration are beating the ammoniacal liquor of 24wt.%, then slurry is mixed with the mixed solvent of 3500mL acetone and ethyl acetate (acetone and ethyl acetate The volume ratio of ester is 3:1) after mixing, obtain reaction raw material mixture;

[0049] (2) The reaction raw material mixture and oxygen are passed into the microchannel reactor for oxidation reaction according to the raw material mixture 2.9mL / min, and the flow velocity of oxygen 14.3mL / min. The reaction temperature is 60°C, the residence time is 3min, and the reaction pressure is 0.25MPa; Microchannel reaction The device is 10 pieces connected in series, the single piece volume is 1.86mL, and the total volume is 18.6mL;

[0050] (3) Distilling the product solution obtained from the reaction under reduced pressure to recover the organi...

Embodiment 2

[0053] A continuous production method of vulcanization accelerator DPG, comprising the steps of:

[0054] (1) beating 700g diphenylthiourea, 0.5g catalyst copper chloride and 680mL concentration of 20wt.% ammonia water, and then mixing the slurry with 8400mL ethyl acetate to obtain a reaction raw material mixture;

[0055] (2) The reaction raw material mixture and oxygen are passed into the pipeline reactor for oxidation reaction according to the flow rate of the raw material mixture 10.5mL / min and oxygen 99mL / min, the reaction temperature is 55°C, the residence time is 3min, and the reaction pressure is 0.1MPa; the volume of the pipeline reactor 150mL;

[0056] (3) Distilling the product solution obtained from the reaction under reduced pressure to recover the organic solvent, and the solid material obtained is washed with alkali, washed with water, and dried to obtain the vulcanization accelerator DPG.

[0057] After calculation, the yield of DPG in this example is 94.9% (b...

Embodiment 3

[0059] A continuous production method of vulcanization accelerator DPG, comprising the steps of:

[0060] (1) beating 700g diphenylthiourea, 0.7g catalyst copper acetate and 1000mL concentration of ammonia water of 15wt.%, then dissolving the slurry into 5600mL of acetone to obtain a reaction raw material mixture;

[0061] (2) The reaction raw material mixture and oxygen are passed into the tower reactor for oxidation reaction according to the flow rate of raw material mixture 5.6mL / min and oxygen 60mL / min, the reaction temperature is 65°C, the residence time is 3min, and the reaction pressure is 0.15MPa; the pipeline reactor The volume is 100mL;

[0062] (3) Distilling the product solution obtained from the reaction under reduced pressure to recover the organic solvent, and the solid material obtained is washed with alkali, washed with water, and dried to obtain the vulcanization accelerator DPG.

[0063] After calculation, the yield of DPG in this example is 95.5% (based on...

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PUM

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Abstract

The invention provides a continuous production method for a vulcanization accelerator DPG. The method comprises the following steps that (1) diphenylthiourea, a catalyst, ammonium hydroxide and an organic solvent are mixed to obtain a reaction raw material mixture; (2) the reaction raw material mixture and an oxidizing agent are subjected to an oxidation reaction in a continuous flow reactor to obtain a reaction product; (3) the reaction product is post-treated to obtain the vulcanization accelerator DPG, wherein the organic solvent in step (1) can dissolve the diphenylthiourea and the vulcanization accelerator DPG. The method reduces the pressure in the reaction process, improves the utilization rate of the raw materials, stabilizes the product quality, greatly shortens the reaction timecompared with a conventional technology, improves the reaction yield, and effectively overcomes the disadvantage of traditional kettle type batch production.

Description

technical field [0001] The invention belongs to the technical field of rubber accelerators, and relates to a continuous production method of a vulcanization accelerator DPG. Background technique [0002] In the process of using rubber to produce various rubber products such as tires, hoses and rubber shoes, five types of additives must be used, which are rubber vulcanization accelerators (referred to as accelerators), rubber antioxidants, rubber vulcanization and vulcanization activators, processing Type rubber additives and special functional additives. The vulcanization accelerator is called accelerator for short. Substances that promote vulcanization. It can shorten the vulcanization time, lower the vulcanization temperature, reduce the amount of vulcanizing agent and improve the physical and mechanical properties of rubber. [0003] The chemical name of the accelerator DPG is 1,3-diphenylguanidine. It is one of the important varieties of rubber vulcanization accelerat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C277/08C07C279/18
CPCC07C277/08C07C279/18
Inventor 孟庆森李霞郝鹏飞
Owner KEMAI CHEM
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