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Process for synthesizing rubber vulcanization accelerator TBBS by electrolytic method in water phase

A technology of vulcanization accelerator and synthetic rubber, applied in the field of electrochemistry, can solve the problems of long reaction time, high production cost, excessive tertiary butylamine, etc., and achieve the effects of easy industrialization and application, simple and environmentally friendly production process, and reduced consumption of raw materials

Active Publication Date: 2014-10-22
JIAXING BEIHUA POLYMER ADDITIVES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sodium hypochlorite method is currently the most used method in industrial production, but it produces a large amount of salty wastewater that is difficult to handle, which seriously pollutes the environment; the hydrogen peroxide method also produces a large amount of low-salt wastewater, and the yield is low; the catalytic oxidation method (oxygen or Air as an oxidant) is a relatively clean method, but it has disadvantages such as long reaction time, high production cost, pressure device, and large investment in equipment; the chlorine oxidation method uses a large amount of tert-butylamine, which has been eliminated by industrial production
[0004] US4127454 has reported the electrolytic oxidation method, prepares TBBS by 2-mercaptobenzothiazole (accelerator M) or disulfide benzothiazole (accelerator DM) and terbutylamine reaction, and solvent is respectively dimethylformamide, acetonitrile, two Polar aprotic solvents such as methyl chloride (perchlorate or halide of metal or quaternary ammonium for the corresponding electrolyte, etc.), protic solvents such as alcohol (metal or ammonium salt of C1-C3 carboxylic acid for the corresponding electrolyte, etc.) and water ( Corresponding electrolytes use hydrochloric acid, sulfuric acid and nitric acid metal salts or hydroxides, etc.), and a mixture of two or three of them can also be used, and the yield can be as high as 99%, but the power consumption is 5-6F / mole, current inefficiency
[0005] The addition of organic solvents to the preparation of TBBS by electrolysis not only reduces the current efficiency, but also brings problems in environmental protection, safety and cost. However, when organic solvents are not used, solids will be precipitated on the anode plate during the electrolysis process, which is difficult to remove by mechanical force. Increase the voltage or decrease the current, reduce the current efficiency, and limit its application in industrial production

Method used

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  • Process for synthesizing rubber vulcanization accelerator TBBS by electrolytic method in water phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Take the raw material 2-mercaptobenzothiazole (accelerator M), tert-butylamine and saturated saline, and make a 2400g suspension in a weight ratio of 1:1.5:10, put it in the electrolytic cell, and place the ultrasonic vibrator in the lower part of the electrolytic cell; The anode is a titanium electrode, the cathode is a nickel electrode, and the electrode is a flat mesh structure with openings; after stirring evenly, cool to 10 o C, connect the DC power supply, the current density is 100 A / m 2 , and then turn on the ultrasonic wave, the ultrasonic frequency is 30kHZ. Samples were taken at intervals of 0.5 h after electrification, and detected by LC. After 6.5 hours of reaction, the conversion rate did not change. Turn off the power, filter, wash, and dry to obtain the rubber accelerator TBBS product. The product yield is 96%, and the current efficiency is 79%.

Embodiment 2

[0016] Take the raw material accelerator M, tert-butylamine and saturated saline, and make 3000g suspension liquid according to the weight ratio of 1:5:50, put it into the electrolytic cell, and place the ultrasonic vibrator on both sides of the electrolytic cell; the anode is iridium-tantalum-coated DSA The electrode, the cathode is made of stainless steel, and the electrode is a flat plate structure; after stirring evenly, cool to 5 o C, connect the DC power supply, the current density is 300 A / m 2 , and then turn on the ultrasonic wave, the ultrasonic frequency is 22kHZ. Samples were taken at intervals of 0.5 h after electrification, and detected by LC. After 4.5 hours of reaction, the conversion rate did not change. Turn off the power, filter, wash, and dry to obtain the rubber accelerator TBBS product. The product yield is 99%, and the current efficiency is 82%.

Embodiment 3

[0018] Take the raw material accelerator M, tert-butylamine and saturated saline, and make 3000g suspension liquid according to the weight ratio of 1:8:80, put it into the electrolytic cell, put the ultrasonic vibrating rod in the internal reaction liquid of the electrolytic cell; the anode is iridium tantalum Coated DSA electrode, the cathode is a platinum electrode, and the electrode is a flat mesh structure with openings; after stirring evenly, cool to 15 o C, connect the DC power supply, the current density is 400 A / m 2 , and then turn on the ultrasonic wave, the ultrasonic frequency is 40kHZ. Samples were taken at intervals of 0.5 h after electrification, and detected by LC. After 4.0 hours of reaction, the conversion rate did not change. The power was turned off, and the rubber accelerator TBBS product was obtained by filtering, washing, and drying. The product yield is 99%, and the current efficiency is 81%.

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Abstract

The invention discloses a new process for producing a rubber vulcanization accelerator TBBS (N-tert-butyl-2-benzothiazole sulfenamide) by an ultrasonic electrolytic method in a water phase, belonging to the field of electrochemistry. The process comprises the following steps: respectively adding 2-mercaptobenzothiazole or sodium salts thereof and tert-butylamine in a weight ratio of 1 to (1.5-10) to an electrolyzer which is filled with a saturated sodium chloride water solution and is provided with ultrasonic vibrators or ultrasonic vibration rods, stirring the materials at 5-15 DEG C, switching on a direct-current power supply, turning off the power supply after electrolytic reaction for a period of time and carrying out filtration, washing and drying, thus obtaining the rubber accelerator TBBS product. The yield of the product is above 96% and the current efficiency is above 79%. The new process has the beneficial effects that the method is simple in process and easily achieves industrialization; organic solvents are not used in the electrolytic process and the electrolyte can be recycled, so that the new process is clean and environment-friendly and environmental pollution and equipment corrosion are reduced.

Description

technical field [0001] The invention relates to a production process of a rubber vulcanization accelerator TBBS, in particular to a new process for synthesizing a rubber vulcanization accelerator TBBS by electrolysis in a water phase, belonging to the field of electrochemistry. Background technique [0002] N-tert-butyl-2-benzothiazole sulfenamide (TBBS) is an important rubber vulcanization accelerator, which has two advantages of scorch resistance and fast vulcanization speed, and is very safe at operating temperature. Produces carcinogenic nitrosamines. It can be used in natural rubber, styrene-butadiene rubber, butadiene rubber, isoprene rubber, etc. It is an ideal replacement product for N-oxydiethylene-2-benzothiazole sulfenamide (NOBS). At present, TBBS has become the leading accelerator variety in the foreign market. In developed countries, the usage of TBBS accounts for about 35%-45% of the total consumption of accelerators, and it shows an increasing trend year by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/00C25B9/00C25B15/08
Inventor 李中贤刘小培王俊伟胡卫东董学亮赵灿方余学军徐丹
Owner JIAXING BEIHUA POLYMER ADDITIVES