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Preparation methods of cumyl peroxyneodecanoate (CNP) and solvent type CNP

A technology of cumyl decanoate and cumene hydroperoxide, which is applied in the field of preparation of cumyl peroxyneodecanoate and solvent-based CNP, can solve the problem of shortening the production cycle, reducing the content of the water phase, and reducing labor Intensity and other issues, to achieve the effect of shortening the production cycle, improving the activity of the initiator, and reducing labor intensity

Active Publication Date: 2020-04-10
鄂尔多斯市瀚博科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] The purpose of the present invention is to overcome the deficiencies in the prior art and provide a kind of preparation method of solvent type cumyl peroxyneodecanoate initiator with high transparency and high activity, effectively solve the problem that cumene hydroperoxide remains in the solvent Type cumyl peroxyneodecanoate initiator causes the problem of decreased activity, effectively reduces the content of the water phase, and then reduces the content of water-soluble ions such as chloride ions, iron ions, sodium ions, and potassium ions. At the same time, a synergist composed of surfactant and antifreeze is added to directly prepare a solvent-based cumyl peroxyneodecanoate initiator with high transparency and high stability, which effectively shortens the production cycle and reduces labor intensity. Increased safety factor and avoid loss of target product

Method used

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  • Preparation methods of cumyl peroxyneodecanoate (CNP) and solvent type CNP

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0080] A kind of preparation method of solvent type cumyl peroxyneodecanoate comprises the steps:

[0081] synthesis:

[0082] (1) 600kg of cumene hydroperoxide is added dropwise in 25% potassium hydroxide lye, the dry basis mass ratio of said lye and cumene hydroperoxide is 0.4:1, the time for adding is 20min, dropwise Stir for 15 minutes after the addition to obtain solution 1;

[0083] (2) Add neodecanoyl chloride dropwise to solution 1, the dry basis mass ratio of cumene hydroperoxide to neodecanoyl chloride is 0.8:1, the dropwise addition time is 45min, after the dropwise addition is completed, react at 25°C for 60min , let it stand for 30 minutes, and divide the water to obtain a water-in-oil emulsion;

[0084] Purification:

[0085] (1) Wash the water-in-oil emulsion with 5% sodium hydroxide solution, the mass ratio of the dry basis of the sodium hydroxide to the water-in-oil emulsion is 0.06:1, leave it standing after washing, divide water, and obtain the solution ...

Embodiment 2

[0093] A kind of preparation method of solvent type cumyl peroxyneodecanoate comprises the steps:

[0094] synthesis:

[0095] (1) 600kg of cumene hydroperoxide is added dropwise in 35% sodium hydroxide lye, the dry basis mass ratio of said lye and cumene hydroperoxide is 0.6:1, the time for adding is 30min, dropwise Stir for 20 minutes after the addition to obtain solution 1;

[0096] (2) Add neodecanoyl chloride dropwise to solution 1, the dry basis mass ratio of cumene hydroperoxide to neodecanoyl chloride is 1.0:1, the dropping time is 60min, after the dropping is completed, react at 35°C for 90min , let it stand for 45 minutes, and divide the water to obtain a water-in-oil emulsion;

[0097] Purification:

[0098] (1) Wash the water-in-oil emulsion with 25% potassium hydroxide solution, the mass ratio of the dry basis of the potassium hydroxide to the water-in-oil emulsion is 0.1:1, leave it standing after washing, divide water, and obtain the solution 2;

[0099] (2...

Embodiment 3

[0106] A kind of preparation method of solvent type cumyl peroxyneodecanoate comprises the steps:

[0107] synthesis:

[0108] (1) 600kg cumene hydroperoxide is added dropwise in 30% potassium hydroxide lye, the dry basis mass ratio of said lye and cumene hydroperoxide is 0.5:1, and the time for adding is 25min, dropwise Stir for 30 minutes after the addition to obtain solution 1;

[0109] (2) Add neodecanoyl chloride dropwise to solution 1, the mass ratio of cumene hydroperoxide to neodecanoyl chloride on a dry basis is 0.9:1, and the dropping time is 50 minutes. After the dropping is completed, react at 30°C for 75 minutes , let it stand for 36 minutes, and divide the water to obtain a water-in-oil emulsion;

[0110] Purification:

[0111] (1) Wash the water-in-oil emulsion with 15% sodium hydroxide solution, the mass ratio of the dry basis of the sodium hydroxide to the water-in-oil emulsion is 0.08:1, leave it standing after washing, divide water, and obtain the solutio...

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Abstract

The invention relates to the technical field of initiators, specifically to preparation methods of cumyl peroxyneodecanoate (CNP) and solvent type CNP. The preparation method of the cumyl peroxyneodecanoate comprises synthesis and purification, wherein cumene hydroperoxide, an alkali liquid and neodecanoyl chloride are subjected to a reaction to obtain a water-in-oil emulsion, the water-in-oil emulsion is washed by adopting four treating agents, and standing and water separating are performed to obtain the cumyl peroxyneodecanoate. According to the invention, the problems that initiating activity reducing and unit consumption increase of a dispersing agent due to the remaining of cumene hydroperoxide in a solvent type cumyl peroxyneodecanoate initiator are effectively solved, and the contents of water-soluble ions such as chlorine ions, iron ions, sodium ions, potassium ions and the like are reduced; and by adding a synergist comprising a surfactant and an anti-freezing agent, the solvent type cumyl peroxyneodecanoate initiator with high transparency and high stability is directly prepared, so that the production period is effectively shortened, the labor intensity is reduced, thesafety coefficient is increased, and the loss of a target product is avoided.

Description

technical field [0001] The invention relates to the technical field of initiators, in particular to a preparation method of cumyl peroxyneodecanoate and solvent-based CNP. Background technique [0002] Cumyl peroxyneodecanoate (CNP), a colorless or pale yellow liquid that flows easily, is mainly used as an initiator for PVC polymerization. The higher the activity of the initiator, the lower the suitable polymerization reaction temperature. The suitable polymerization reaction temperature range of cumyl peroxyneodecanoate is 40-60°C, and the content can still be kept at a certain level when stored below -15°C for a long time. Change. [0003] With the rapid development of the domestic polymer synthesis industry, the variety and demand of initiators for polymer synthesis have increased rapidly. Solvent-based cumyl peroxyneodecanoate is used as a high-efficiency initiator for polymer synthesis. In the polymerization process, the dosage is small, and it is easy to disperse in ...

Claims

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Application Information

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IPC IPC(8): C07C409/38C07C407/00C08F4/34C08F114/06
CPCC07C407/003C07C407/00C08F4/34C08F114/06C07C409/38
Inventor 赵长森王会昌张强查美琴王鑫龙颜艺专牛强
Owner 鄂尔多斯市瀚博科技有限公司
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