Dicumyl peroxide production method

A technology of dicumyl peroxide and its production method, which is applied to the preparation of peroxide compounds, chemical instruments and methods, and the preparation of organic compounds. Eliminate the problems of low yield of granular crystals, and achieve the effects of perfect crystal growth, reduced occlusion and coalescence, and reduced operation difficulty

Active Publication Date: 2019-04-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problems to be solved by the present invention are poor product quality, irregular crystal shape, poor transparency, serious crystal occlusion and coalescence, uneven distribution of crystal particle size, and large grain crystals in the existing dicumyl peroxide production method. The problems of low yield and high production energy consumption provide a method for producing dicumyl peroxide

Method used

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  • Dicumyl peroxide production method

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Effect test

Embodiment 1

[0023] The production method of dicumyl peroxide of the present invention.

[0024] Such as figure 1 Described, the 90% raw material that contains dicumyl peroxide concentration is carried out cooling crystallization in the crystallizer with crystallization solvent (95% ethanol), adds crystal seed when being down to saturation temperature, and seed crystal amount is diisopropyl peroxide 10% of the amount of benzene raw material, the purity of the seed crystals is 99.5%, the particle size is 710 μm, the heat transfer temperature difference is controlled to be 3°C, and the crystallization end point temperature is 2°C to obtain crystal slurry I containing dicumyl peroxide crystals; I carry out solid-liquid separation to obtain dicumyl peroxide crystals I and crystallization mother liquor I, and the crystallization mother liquor I is discharged from the crystallization device for solvent recovery; the dicumyl peroxide crystals I are sent into the beating tank, and saturated crysta...

Embodiment 2

[0026] The production method of dicumyl peroxide of the present invention.

[0027] Such asfigure 1 As described above, according to the operation method of Example 1, the crystallization process is continuous crystallization, only adding seed crystals during the start-up stage, the crystallization temperature is 5°C, the temperature difference of heat transfer is controlled to be 5°C, and the particle size of dicumyl peroxide crystal I The fine powder of ≤425μm accounts for 15%. The operating temperature of beating and washing is 7°C. Crystal I loses 15% of its mass due to beating and washing. Part of the crystallization mother liquor II is returned to the beating tank as washing liquid, and the rest is returned to the crystallizer to continue crystallization. The dicumyl peroxide product is finally obtained. The product is a granular crystal, regular in shape, transparent, free of occlusion and agglomeration, with a purity of 99.9%. The crystal particle size distribution is u...

Embodiment 3

[0029] The production method of dicumyl peroxide of the present invention.

[0030] Such as figure 1 As described above, according to the operation method of Example 1, the crystallization solvent is absolute ethanol, the crystallization process is continuous crystallization, only adding seed crystals during the start-up stage, the crystallization temperature is 0°C, the heat transfer temperature difference is controlled to be 2°C, diisoperoxide The fine powder with a particle size of ≤425μm accounts for 10% of the propylbenzene crystal I. The operating temperature for beating and washing is 3°C. The crystal I loses 10% of its mass due to beating and washing. Part of the crystallization mother liquor II is returned to the beating tank as washing liquid, and the rest is returned to the beating tank. Continue to crystallize in the crystallizer, and finally obtain the product of dicumyl peroxide. The product is a granular crystal, regular in shape, transparent, free of occlusion ...

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Abstract

The invention relates to a dicumyl peroxide production method, which comprises: co-feeding a dicumyl peroxide raw material and a crystallization solvent into a crystallizer, carrying out cooling crystallization, and carrying out solid-liquid separation on the obtained crystal slurry to obtain a dicumyl peroxide crystal I and a crystallization mother liquor I; discharging the crystallization motherliquor I out of the crystallization device, and carrying out solvent recovery; feeding the dicumyl peroxide crystal I into a beating washing tank, and carrying out beating washing on the dicumyl peroxide crystal I by using a washing liquid; carrying out solid-liquid separation on the obtained crystal slurry to obtain a dicumyl peroxide crystal II and a crystallization mother liquor II; drying thedicumyl peroxide crystal II, and discharging as the product; and returning the crystallization mother liquor II to the crystallizer, and continuously crystallizing. According to the present invention, the dicumyl peroxide production method can solve the problems of poor product quality, irregular crystal shape, poor transparency, serious crystal occlusion and coalescence, non-uniform size and non-uniform distribution of crystal particles, low yield of large particle crystals and high energy consumption in the prior art, and can be used in the production of dicumyl peroxide.

Description

technical field [0001] The invention relates to a production method of dicumyl peroxide. Background technique [0002] Dicumyl peroxide is a strong oxidizing agent, referred to as DCP. It is mainly used as a vulcanizing agent for natural rubber and synthetic rubber, an initiator for polymerization reactions, and can also be used as a crosslinking agent for polyethylene resin. It is widely used in shoemaking , wire and cable and building materials and rubber industries. [0003] The production of dicumyl peroxide mainly adopts the batch crystallization method at present, and existing problems include: 1) product quality is relatively poor, such as inhomogeneous crystal particle size distribution, fine powder is more, and the yield of large particle crystal product is low, crystal Severe agglomeration, irregular shape, low crystal transparency, internal occlusion, etc.; 2) The fine powder produced in the crystallization process needs to be dissolved and recrystallized again, ...

Claims

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Application Information

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IPC IPC(8): C07C409/16C07C407/00
CPCC07C407/003C07C409/16
Inventor 陈亮张杰蔡立鑫郭艳姿
Owner CHINA PETROLEUM & CHEM CORP
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