A kind of preparation method of emulsion type cumyl peroxyneodecanoate

A technology of cumyl decanoate and cumene hydroperoxide, which is applied in the field of preparation of emulsion-type cumyl peroxyneodecanoate, can solve problems such as content reduction, decreased triggering activity, and increased unit consumption. To achieve the effect of enhancing the activity

Active Publication Date: 2021-11-26
鄂尔多斯市瀚博科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The purpose of this invention is to overcome the deficiencies in the prior art and provide a kind of preparation method of high-purity high-activity emulsion type cumyl peroxyneodecanoate initiator, effectively solve the problem that cumene hydroperoxide remains in the emulsion type The problem of decreased initiation activity and increased unit consumption caused by the cumyl peroxyneodecanoate initiator effectively reduces the content of the water phase, thereby reducing the water-soluble ions such as chloride ions, iron ions, sodium ions, and potassium ions The content of the emulsion type cumyl peroxyneodecanoate initiator of high purity and high activity is finally prepared

Method used

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  • A kind of preparation method of emulsion type cumyl peroxyneodecanoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] A kind of preparation method of emulsion type cumyl peroxyneodecanoate comprises the steps:

[0071] synthesis:

[0072] (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;

[0073] (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;

[0074] Purification:

[0075] (1) Wash the water-in-oil emulsion 1 time 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, Obtain solution ...

Embodiment 2

[0082] A kind of preparation method of emulsion type cumyl peroxyneodecanoate comprises the steps:

[0083] synthesis:

[0084] (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;

[0085] (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;

[0086] Purification:

[0087] (1) Wash the water-in-oil emulsion 2 times with 25% sodium sulfite solution, the mass ratio of the dry basis of the sodium sulfite to the water-in-oil emulsion is 0.1:1, leave it to stand after each washing, and divide the water to obtain the solution 2;

...

Embodiment 3

[0094] A kind of preparation method of emulsion type cumyl peroxyneodecanoate comprises the steps:

[0095] synthesis:

[0096] (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;

[0097] (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;

[0098] Purification:

[0099] (1) Wash the water-in-oil emulsion 2 times with 15% sodium bisulfite solution, the dry basis of the sodium bisulfite and the mass ratio of the water-in-oil emulsion are 0.08:1, leave standstill after each washing , divided into water ...

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Abstract

The invention relates to the technical field of initiators, in particular to a method for preparing emulsion-type cumene neodecanoate. The preparation method includes three steps of synthesis, purification and preparation, using cumene hydroperoxide, alkali liquid and neodecanoyl chloride to obtain a water-in-oil emulsion, and then three kinds of treatment agents are used to wash the water-in-oil emulsion, stand still, and separate water to obtain the product. The present invention effectively solves the problem of decreased initiation activity and increased unit consumption of dispersant caused by the residue of cumene hydroperoxide in the emulsion-type cumyl peroxyneodecanoate initiator, and effectively reduces the content of the water phase at the same time. Furthermore, the contents of water-soluble ions such as chloride ions, iron ions, sodium ions, and potassium ions are reduced, and a high-purity and high-activity emulsion-type cumyl peroxyneodecanoate initiator is finally prepared.

Description

technical field [0001] The invention relates to the technical field of initiators, in particular to a preparation method of emulsion type cumyl peroxyneodecanoate. 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. Emulsion-type cumyl peroxyneodecanoate, as a high-efficiency initiator for polymer synthesis, compared with solvent-based initiators, has the same amount of solvent-based initiators in the po...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F14/06C08F4/34
CPCC08F14/06C08F4/34
Inventor 赵长森颜艺专王鑫龙黄亮东查美琴王会昌牛强
Owner 鄂尔多斯市瀚博科技有限公司
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