Method and apparatus for producing benzoyl peroxide

 

The invention relates to a technology for benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium under stirring and cooling. The process is conducted in a continuous circulation of the reaction mixture through the reaction zone and cooling zone. Circulation is subjected to the liquid phase of the reaction mixture after the separation from it of the solid phase by filtration. A device for receiving peroxide benzoyl includes a reactor with a stirrer and a jacket for cooling, means for supplying reagents, a circulation pump, a refrigerator and a filter. The latter preferably is located on the suction side of the circulation pump is immersed in the reactor. The technical result - the simplification of the process while improving the quality characteristics of the final product. 2 S. and 1 C.p. f-crystals, 1 Il.

The invention relates to the chemical industry, and more specifically to methods for producing benzoyl peroxide, used in the manufacture of plastics, rubber, paints and varnishes, adhesive compositions and other industries.

Known methods for producing benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in water sell the 409/34, 407/00, 1997). In these methods, the benzoyl chloride is dosed in an alkaline solution of hydrogen peroxide at a speed that facilitates the removal of a large amount of heat. While benzoyl peroxide get suspended in the reaction mass of solid particles, in particular granules, which is separated from the liquid with known methods, washed, dried and used usually in the form of a granular product having a substantial moisture content, because of dry benzoyl peroxide explosive.

The closest to the invention is a method of obtaining benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium under stirring and cooling in continuous circulation of the reaction mixture through a reaction zone and a cooling zone with a speed not less than 8 recyclo the reaction mass for a single process (EN 2072988, C 07 C 407/00,409/34, 1997).

The known device for obtaining benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium, representing various modifications of the reactor with an agitator and means for cooling (FR 1329593, 07, 1963; DE 1768199, C 07 C 179/14, 1975; JP 52-153926, C 07 C 179/14, 1977; EN 2074178, C 07 C 409/34, 407/00, 1997).

The most the of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium, includes a reactor with a stirrer and a jacket for cooling, circulating pump and a refrigerator (EN 2072988, C 07 C 407/00, 409/34, 1997).

When using the method and devices that are closest to the proposed, due to the intense heat in the cooling zone, external to the reaction zone, is achieved by reducing the duration of the process and the implementation of synergies for about 1 hour. However, benzoyl peroxide is formed in the form of very small particles, which creates certain difficulties in its subsequent filtering (high resistance filterable mass), drying and storage (dusting and the possibility of freezing in the case of storage at temperatures below 0oC). In addition, this method does not exclude the possibility of accumulation of particles of benzoyl peroxide in stagnant areas of the circulation loop that creates the risk of explosion during a long stopover and drying particles that may have accumulated.

To create an intensive process of obtaining benzoyl peroxide in the form of granules method for obtaining benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium under stirring and cooling in continuous circulation of the reaction mixture pension, separated from the solid phase by filtration.

Also proposed a device for receiving benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium, comprising a reactor with a stirrer and a jacket for cooling, means for supplying reagents, circulation pump and refrigerator, characterized in that it further comprises a filter. Preferably, the filter was located on the suction side of the circulation pump is immersed in the reactor, i.e., designed as a submersible filter, as in this case, the filtering surface is constantly washed by stirring the reaction mass, and the problems associated with the need for periodic cleaning, do not occur.

The technical result of the use of the proposed method and device is to provide opportunities for benzoyl peroxide in the form of granules within as short or even shorter than in the known method, time. It turned out that the process under the proposed method in the proposed device does not require the same as in the known method, the number recyclo, and the resulting product contains unreacted benzoyl chloride not more, the specific embodiment of the proposed device, and the following examples 1-3, describing the conduct of the proposed method in this device.

In accordance with the drawing device to obtain benzoyl peroxide consists of a vertical cylindrical reactor 1 with a stirrer and a jacket for cooling, standard 2, 3, 4 and 5 (means for supplying reagents), the circulation pump 6, the refrigerator 7 and filter 8. The latter is put into the reactor 1 the initial part of the suction pipe of the pump 6. The discharge line of the pump 6 is connected to the suction inlet tube space of the refrigerator 7, and the outlet pipe space of the refrigerator 7 - with a pipe in the upper part of the reactor 1.

Example 1. In enameled reactor 1 with a capacity of 2.5 m3equipped with a mixer (mixing speed of 60 rpm), jacketed for cooling the brine and submersible filter 8 connected to the suction inlet of the circulating pump 6, load 1100 kg of demineralized water from the measuring device 2 and 185 kg 42% aqueous sodium hydroxide solution from the measuring device 3. Include a pump 6, which results in continuous fluid circulation (the circulation rate of 12 m3/h) through the reactor 1 and the refrigerator 7 (heat transfer surface 25 m2oWith the reactor from the measuring device 4 add 95 kg 38% aqueous solution of hydrogen peroxide with such speed that the temperature in the reactor did not exceed +4oC. Upon completion of addition of the hydrogen peroxide solution is introduced into the reactor 50 g sultanol and start adding benzoyl chloride from the measuring device 5. For 30 min in the reactor 1 is injected 260 kg of benzoyl chloride, continuing the flow of brine in the jacket of the reactor and refrigerator. The temperature in the reactor does not exceed +4oC. the Number recyclo the reaction mass during the process is about 4. After the introduction of benzoyl chloride circulation and the flow of brine in the refrigerator stop. The reaction mass, which was an aqueous suspension of benzoyl peroxide, is kept in the reactor under stirring for 30 min, and then filtered, washed precipitate on the filter with demineralized water until neutral and dried to a residual moisture content of 25% (wt.). Get 280,7 kg of product with a particle size of 1-3 mm, the mass fractions of the basic substance (in terms of dry product) of 98.5% and a total chlorine content (the value of which is judged on the content of benzoyl chloride in the product) of 0.13%. Output 94,0% of theory.

Example 2. The process is carried out analogously to example 1 with the sup>/h) number recyclo the reaction mass during the process is about 6. Get 285,4 kg of product with a moisture content of 26%, a particle size of 1-3 mm, the mass fractions of the basic substance (in terms of dry product) of 98.5% and a total chlorine content of 0.11%. Output to 94.3% of theory.

Example 3. The process is carried out analogously to example 1 with the difference that the benzoyl chloride added dropwise within 60 minutes, the circulation lead with a speed of 9 m3/h (number recyclo the reaction mass during the process is 6.5). Get 284,5 kg of product with a moisture content of 26%, a particle size of 1-2 mm, the mass fractions of the basic substance (in terms of dry product) of 98.3% and a total chlorine content of 0.11%. Output 94,0% of theory.

Claims

1. The way to get benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide in aqueous-alkaline medium under stirring and cooling in continuous circulation of the reaction mixture through a reaction zone and a cooling zone, wherein the circulation is subjected to the liquid phase of the reaction mixture is separated from the solid phase by filtration.

2. Device to obtain benzoyl peroxide interaction of benzoyl chloride with hydrogen peroxide is in, the circulation pump and refrigerator, characterized in that it further comprises a filter.

3. The device according to p. 2, characterized in that the filter is on the suction side of the circulation pump is immersed in the reactor.

 

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