A kind of crystallization method of large particle dicumyl peroxide

A technology of dicumyl peroxide seed crystals and dicumyl peroxide, which is applied to the preparation of peroxide compounds, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems affecting centrifugation and drying, and crystallization of particles Irregularity, affecting the purity of DCP, etc., to improve crystallization production efficiency, facilitate crystal growth, and improve economic benefits

Inactive Publication Date: 2020-02-07
CHINA PETROLEUM & CHEM CORP
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

2) Slow down the cooling rate, the cooling rate is too fast is the main cause of too large solution saturation and too fast crystallization speed
This document only improves the process of DCP crystallization feeding method, cooling rate and crystallization end point temperature, and does not involve the description of DCP large-grain crystal particles, and crystallize according to the above-mentioned process, most of the DCP obtained are fine powders, and the particles are crystallized. The shape is also irregular, affecting the subsequent centrifugation and drying
Disadvantages: 1) The crystallization solvent is usually industrial alcohol, and the water content of industrial alcohol is at least 5%. At the same time, in the process of alcohol recycling, due to the azeotropic phenomenon of alcohol, water and cumene, water is usually used to remove alcohol from It is extracted from the crystallization mother liquor and distilled, so the water content of the alcohol will increase greatly and can reach 8-15%. Therefore, the DCP fine powder contains a large amount of water-containing alcohol solvent before drying, so it is quite difficult to dry and remove the solvent. DCP There will also be trace solvents in it, which will affect the purity of DCP
2) Even if the DCP obtained by this crystallization process has particles, and due to the particles produced by agglomeration, the crystal form is very poor and fragile
3) Due to the small size of DCP fine powder, it is easy to absorb moisture and agglomerate, which is extremely inconvenient for downstream customers to use

Method used

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  • A kind of crystallization method of large particle dicumyl peroxide
  • A kind of crystallization method of large particle dicumyl peroxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] DCP extraction and concentration liquid is about 2308g (wherein, DCP content is 89.77%, cumene content is 7.69%, p-cumyl benzyl alcohol content is 0.83%, cumene hydroperoxide=0.10%, acetophenone content is 1.0%, α - MS content 0.71%) and industrial alcohol 1731g (the mass ratio of dicumyl peroxide liquid and alcohol solvent is 1:0.75, the mass concentration of industrial alcohol is 88.3%) mix evenly, heat up to 40.74 ℃, control the temperature according to the program Speed, first lower the temperature for 1h40min to reach 29.80℃, then slowly lower the temperature for 1h to 27.50℃, add dicumyl peroxide seed crystals (700-830μm in particle size) and dicumyl peroxide fine powder (with a particle size of 150~550μm), the amount of dicumyl peroxide seed crystals and dicumyl peroxide fine powder is calculated as a percentage of the concentration of the liquid, and the amount of dicumyl peroxide seed crystals is 138g (mass ratio is about 5.98%), the addition of dicumyl peroxid...

Embodiment 2

[0041] The DCP extraction and concentration liquid is about 2362g (wherein, DCP content is 92.02%, cumene content is 5.69%, p-cumyl alcohol content is 0.83%, cumene hydroperoxide=0.10%, acetophenone content is 0.65%, α -MS content 0.71%) and industrial methanol 1420g (the mass percentage of dicumyl peroxide liquid and alcohol solvent is 1:0.6, the mass concentration of industrial methanol is 97.5%) mix evenly, heat up to 40.28 ℃, firstly, cool down for 1h30min The temperature of the crystallization kettle reaches 30.34°C, then slowly lowers the temperature for 1h20min to 27.85°C, and adds dicumyl peroxide seed crystals (700-800 μm in particle size) and dicumyl peroxide fine powder (150-450 μm in particle size), The dicumyl peroxide crystal seed crystal seed and dicumyl peroxide fine powder add-on are the ratio percentage meter of extracting and concentrating the combined liquid, and the dicumyl peroxide crystal seed crystal add-on is 94.48g (mass ratio is about 4%), The added ...

Embodiment 3

[0043] The DCP extraction and concentration liquid is about 2460g (wherein, DCP content is 85.03%, cumene content is 8.96%, p-cumyl alcohol content is 3.04%, cumene hydroperoxide=0.23%, acetophenone content is 1.65%, α -MS content 1.09%) and industrial isopropanol 1355g (the mass percentage of dicumyl peroxide liquid and alcohol solvent is 1:0.55, the mass concentration of industrial isopropanol is 93.6%) mix uniformly, heat up to 49.46 ℃, First, cool down the temperature of the crystallization kettle for 1h50min to 31.65°C, then slowly cool down for 2h to 28.02°C, add dicumyl peroxide seed crystals (with a particle size of 800-830 μm) and dicumyl peroxide fine powder (with a particle size of 450 ~550 μm), the amount of dicumyl peroxide seed crystals and dicumyl peroxide fine powder is the percentage of the concentration and liquid ratio, and the amount of dicumyl peroxide seed crystals is 118g (mass ratio is about 4.8 %), the addition of dicumyl peroxide fine powder is 26g (m...

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Abstract

The invention especially relates to a crystallization method for large-particle dicumyl peroxide, belonging to the technical field of crystallization of dicumyl peroxide. The crystallization method comprises the following steps: 1) uniformly mixing dicumyl peroxide liquid with an alcoholic solvent so as to obtain a mixed solution; and 2) adding a dicumyl peroxide seed crystal and fine dicumyl peroxide powder into the mixed solution obtained in the step 1), and carrying out cooling crystallization to obtain large-particle dicumyl peroxide. According to the preparation method, the addition of the dicumyl peroxide seed crystal and the fine dicumyl peroxide powder is beneficial for crystal growth and effective inhibition of the generation of fine powder; and the yield of large-particle dicumylperoxide in a prepared dicumyl peroxide product is as high as 95% or above.

Description

technical field [0001] The invention relates to the technical field of crystallization of dicumyl peroxide, in particular to a crystallization method of large particle dicumyl peroxide. Background technique [0002] Dicumyl peroxide (DCP) is an organic peroxide crosslinking agent, mainly used as a crosslinking agent for various olefin polymers and copolymers (such as polyethylene, chlorinated polyethylene, silicone rubber, etc.) As well as a polymerization initiator for polystyrene, it can also be used as a curing agent for unsaturated polyester resins, which exhibits very useful properties and is widely used. However, if a small amount of impurities is contained in DCP, it will adversely affect the polymerization reaction, and cause coloring and deterioration of physical properties of the produced polymer. Therefore, higher purity DCP is required. In recent years, there has been a tendency to demand improvement of work efficiency or improvement of work environment. DCP i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C407/00C07C409/16
CPCC07C407/003C07C409/16
Inventor 崔敏华傅跃华谭永生徐卫民许耀新
Owner CHINA PETROLEUM & CHEM CORP
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