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System and preparation method for preparing accelerant N,N'-thiocarbanilide via continuous reaction

A technology of diphenylthiourea and accelerator, which is applied in the field of continuous reaction preparation of accelerator N, can solve the problems of reaction product yield influence, environmental pollution, waste liquid discharge, etc., achieves small footprint, saves water resources, The effect of high reaction efficiency

Active Publication Date: 2019-02-22
BEIJING RED AVENUE INNOVA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The above methods all have common disadvantages: first, these reactions are carried out in a heterogeneous system where an organic phase and an aqueous phase coexist, and the reactants are contacted as fully as possible by means of surfactants or ultrasound to achieve the purpose of sufficient reaction. The yield of the reaction product of the homogeneous reaction system will inevitably be affected; secondly, most of the reactions are carried out under alkaline conditions, and by-products such as sodium salts will be generated, which must be washed to remove the salt. water, which will inevitably cause the discharge of waste liquid and the pollution of the environment

Method used

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  • System and preparation method for preparing accelerant N,N'-thiocarbanilide via continuous reaction
  • System and preparation method for preparing accelerant N,N'-thiocarbanilide via continuous reaction
  • System and preparation method for preparing accelerant N,N'-thiocarbanilide via continuous reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] (1) adding sulfur to carbon disulfide according to mass fraction 2% to completely dissolve sulfur;

[0053] (2) Aniline and carbon disulfide / sulfur are injected through a high-pressure plunger pump at the same time with a flow rate of 27ml / min and 10ml / min respectively, fully mixed through an in-line mixer, and then entered into a steel tubular reactor with an internal diameter of 2cm to react, The length of the tubular reactor is 18m, the temperature of the tubular reactor is 200°C, and the internal pressure of the tubular reactor is maintained at 5MPa;

[0054] (3) The reaction solution flows forward under the push of the high-pressure plunger pump, and exits the tubular reactor after about 150 minutes;

[0055] (4) After the gas hydrogen sulfide produced by the reaction comes out from the tubular reactor, it enters the gas storage tank and is directly absorbed with sodium hydroxide lye;

[0056] (5) After the liquid component produced by the reaction comes out of th...

Embodiment 2

[0061] (1) adding sulfur to carbon disulfide according to 5% by mass fraction to completely dissolve the sulfur;

[0062] (2) Inject aniline and carbon disulfide / sulfur into a high-pressure plunger pump at the same time at a flow rate of 55ml / min and 35ml / min respectively, mix fully through an online mixer, and then enter a steel tubular reactor with an inner diameter of 3cm for mixed reaction , the length of the tubular reactor is 25m, and the temperature of the tubular reactor is heated at 175°C; the internal pressure of the tubular reactor is maintained at 7MPa;

[0063] (3) The reaction solution flows forward under the push of the high-pressure plunger pump, and exits the tubular reactor after about 200 minutes;

[0064] (4) After the gas hydrogen sulfide produced by the reaction comes out from the tubular reactor, it enters the gas storage tank and is directly absorbed with sodium hydroxide lye;

[0065] (5) After the liquid component produced by the reaction comes out o...

Embodiment 3

[0069] (1) Inject aniline and carbon disulfide through a high-pressure plunger pump at the same time at flow rates of 60ml / min and 40ml / min respectively, mix thoroughly through an online mixer, and then enter a steel tubular reactor with an inner diameter of 2cm for reaction. The length of the reactor is 48m, and the temperature of the heated tubular reactor is 250°C; the internal pressure of the tubular reactor is maintained at 7MPa;

[0070] (2) The reaction solution flows forward under the push of the high-pressure plunger pump, and exits the tubular reactor after about 150 minutes;

[0071] (3) After the gas hydrogen sulfide produced by the reaction comes out from the tubular reactor, it enters the gas storage tank and is directly absorbed with sodium hydroxide lye;

[0072] (4) After the liquid component produced by the reaction comes out of the tubular reactor, it enters the product receiving tank, and ethyl acetate solvent is added, and the product N, N'-diphenylthioure...

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Abstract

The present invention relates to a system and preparation method for preparing an accelerant N,N'-thiocarbanilide via continuous reaction in the field of rubber vulcanization. The system and method can achieve continuous uninterrupted reaction with high production efficiency; compared with the traditional preparation method, the reaction is carried out in a completely organic phase, and the reactants can be sufficiently contacted, so that fewer reaction by-products are caused, no waste water is generated, and no sodium is produced, a water washing process is not required, and a lot of water resources are saved; the whole process of the reaction is carried out in a closed link, the unreacted carbon disulfide and aniline and the sulfur produced by the treatment of hydrogen sulfide in an incinerator can be returned for reuse, recycling and energy saving properties are provided, and the whole process is cleaning, so that the preparation process is more efficient and environmentally friendly and accords with the current national industrial upgrading trend.

Description

technical field [0001] The invention relates to the field of rubber vulcanization, and furthermore, relates to a system and a preparation method for continuous reaction preparation of accelerator N, N'-diphenylthiourea. Background technique [0002] The vulcanization accelerator can greatly accelerate the reaction between rubber and vulcanizing agent during the vulcanization process of rubber, thereby improving productivity, and can also improve the mechanical properties of the rubber compound. With the development of the rubber industry, the research and production of rubber vulcanization accelerators have attracted more and more attention. N, N'-diphenylthiourea, referred to as diphenylthiourea or DPTU, is a medium-speed vulcanization accelerator for natural rubber and synthetic rubber. It is mainly used for natural latex and neoprene latex products, and can also be used for Manufacture of vulcanization bladders, water tires, tire sealants, wires and cables, industrial pr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C335/16
CPCC07C335/16
Inventor 张洁阮振刚张成董栋张宁
Owner BEIJING RED AVENUE INNOVA
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