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A kind of crystallization method of large particle dicumyl peroxide

A technology of dicumyl peroxide seed crystal seed and dicumyl peroxide, which is applied in the preparation of peroxy compounds, chemical instruments and methods, preparation of organic compounds, etc. and drying, affecting the purity of DCP, etc., to achieve the effect of good crystal shape, reducing the amount of fine powder and high solute yield

Active Publication Date: 2021-06-11
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] The DCP extraction and concentration liquid is about 4.1 tons (wherein, dicumyl peroxide: 89.46wt%, dimethyl benzyl alcohol: 1.36wt%, cumene hydroperoxide: 0.15wt%, acetophenone: 0.98 wt%, cumene: 7.13wt%, α-MS: 0.92wt%) and 2.38 tons of industrial alcohol (the mass ratio of dicumyl peroxide liquid and alcohol solvent is 1:0.58, and the mass concentration of industrial alcohol is 85.3 wt%) mix uniformly, heat up to 49.6°C, control the cooling rate according to the program, at first the mixed solution obtained in step 1) is cooled to 37.7°C at a cooling rate of 3.8°C / h, add 0.062 tons of water (water is 2.6wt of industrial alcohol %); the mixed solution after adding water is cooled to 29.7 ℃ with 3 ℃ / h cooling rate, then adds dicumyl peroxide crystal seed (particle size is 700 ~830 μm) and dicumyl peroxide fine powder (particle size is 150~550 μm), the addition amount of dicumyl peroxide seed crystal and dicumyl peroxide fine powder is calculated as the ratio percentage ...

Embodiment 2

[0043] The DCP extraction and concentration liquid is about 4.0 tons (wherein, DCP: 92.32wt%, cumene: 5.06wt%, dimethyl benzyl alcohol: 1.08wt%, cumene hydroperoxide: 0.59wt%, acetophenone : 0.30wt%, α-MS: 0.65wt%) and 2.6 tons of industrial methanol (the mass ratio of dicumyl peroxide liquid and alcohol solvent is 1:0.65, and the mass concentration of industrial methanol is 98.6wt%) mix homogeneously, Be warming up to 40.2 DEG C, control the cooling rate according to the program, first the mixed solution obtained in step 1) is cooled to 30.4 DEG C at a cooling rate of 4.5 DEG C / h, add 0.242 tons of water (water is 9.3% of industrial methanol); The mixed solution was cooled to 30.9 °C at a cooling rate of 6 °C / h, and then cooled to 28.8 °C at a cooling rate of 1.5 °C / h. Cumene fine powder (particle size: 150-550 μm), dicumyl peroxide seed crystals and dicumyl peroxide fine powder additions are calculated as percentages of the concentration and liquid mixture, dicumyl peroxide ...

Embodiment 3

[0045] The DCP extraction and concentration liquid is about 3.8 tons (wherein, DCP: 85.05%, dimethyl benzyl alcohol: 2.24%, cumene hydroperoxide: 0.72%, acetophenone: 1.61%, cumene: 8.86%, α-MS: 1.52%) mixes homogeneously with 2.85 tons of industrial isopropanol (the mass ratio of dicumyl peroxide liquid and alcohol solvent is 1:0.75, and the mass concentration of industrial isopropanol is 90.1wt%), is heated up to 45.7°C, control the cooling rate according to the program, first the mixed solution obtained in step 1) is cooled to 33.8°C at a cooling rate of 5.7°C / h, and 0.222 tons of water (water is 7.8% of industrial isopropanol) is added; The mixed solution was cooled to 29.1 °C at a cooling rate of 5 °C / h, and then cooled to 26.2 °C at a cooling rate of 1 °C / h, and then dicumyl peroxide seed crystals (particle size 700-830 μm) and di Cumene fine powder (particle size: 150-550 μm), dicumyl peroxide seed crystals and dicumyl peroxide fine powder additions are calculated as pe...

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Abstract

The invention relates to the technical field of crystallization of dicumyl peroxide, in particular to a crystallization method of large particle dicumyl peroxide. The crystallization method comprises the following steps: 1) uniformly mixing dicumyl peroxide liquid and alcohol solvent to obtain a mixed solution; 2) adding water and dicumyl peroxide seed crystals to the mixed solution obtained in step 1) and dicumyl peroxide fine powder, crystallized by cooling to obtain the large particle dicumyl peroxide. The preparation method of the present invention adds water, dicumyl peroxide seed crystals and dicumyl peroxide fine powder, which is beneficial to crystal growth and effectively inhibits the generation of fine powder, and large particles in the prepared dicumyl peroxide product The yield of dicumyl peroxide is high, and the yield in industrial production can reach more than 85%.

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
Inventor 崔敏华谭永生杨骅徐卫民许耀新徐裕傅跃华
Owner CHINA PETROLEUM & CHEM CORP
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