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A kind of immobilized phase-transfer catalyst and its application in the preparation of cumyl peroxy neodecanoate

A technology of phase transfer catalyst and cumene hydroperoxide, which is applied in the direction of physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, peroxygen compound preparation, etc., which can solve the inefficient separation of mother liquor and water and other problems, to achieve the effect of stable product quality, convenient operation and short process time

Inactive Publication Date: 2019-11-29
鄂尔多斯市瀚博科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] For the deficiencies in the technical field, the object of the present invention is to provide a kind of immobilized phase-transfer catalyst, to solve the inefficient problem of mother liquor and water separation in the production process of neodecanoyl peroxide

Method used

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  • A kind of immobilized phase-transfer catalyst and its application in the preparation of cumyl peroxy neodecanoate
  • A kind of immobilized phase-transfer catalyst and its application in the preparation of cumyl peroxy neodecanoate
  • A kind of immobilized phase-transfer catalyst and its application in the preparation of cumyl peroxy neodecanoate

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Effect test

Embodiment 1

[0032] Prepare the tetramethylammonium bromide phase transfer catalyst with MCM-41 as the carrier: add 2.2g tetramethylammonium bromide and 40ml isopropanol in a 150ml three-necked bottle equipped with a reflux condenser and a thermometer, stir at room temperature 0.5h, mix evenly, then add 3.4g MCM-41, reflux and stir for 15h under heating, filter while hot, wash with water until neutral, dry at 80°C for 10h, and obtain the phase transfer of tetramethylammonium bromide immobilized Catalyst, labeled (TMAC)-MCM-41.

[0033] In the preparation reaction of cumyl peroxy neodecanoate, it is recycled 48 times, and its recycling stability index is as follows figure 1 shown.

Embodiment 2

[0035] Prepare the hexaalkyltrimethylammonium bromide phase-transfer catalyst with SBA-15 as the carrier: add 2.9g tetramethylammonium bromide and 45ml ethanol in the 150ml three-necked bottle that reflux condenser, thermometer are housed, at room temperature Stir for 1h, mix well, then add 4.2g of SBA-15, stir for 20h under heating and reflux conditions, filter while hot, wash with water until neutral, and dry at 80°C overnight to obtain immobilized hexaalkyltrimethyl Ammonium bromide phase transfer catalyst, labeled (HTMAC)-SBA-15.

[0036] After the catalyst is recycled 46 times in the preparation reaction of cumyl peroxynedecanoate, the yield of the finished product still reaches 96%. Its recycling stability indicators such as figure 2 shown.

Embodiment 3

[0038] Preparation of 15-crown-5 ether phase transfer catalyst with styrene-divinylbenzene copolymer as carrier: add 3.3g of 15-crown-5 ether and 40mL toluene in a 150ml three-necked bottle equipped with a reflux condenser and a thermometer , stirred at room temperature for 0.5h, then added 4.8g of styrene-divinylbenzene copolymer, heated under reflux and stirred for 10h, filtered while hot, and dried under vacuum at 80°C overnight to obtain the immobilized 15-crown-5 phase transfer Catalyst, labeled (POCPD)-PSD.

[0039] In embodiment 5, the yield of cumyl peroxy neodecanoate preparation reaction is recycled 36 times and the yield is 93%, and its recycling stability index is as follows: image 3 shown.

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Abstract

The invention provides an immobilized phase transfer catalyst which is prepared by the following methods: adding a carrier into an organic solvent containing a phase transfer catalyst, performing heating reflux, performing a reaction for 10-20h, washing and filtering, so as to obtain the immobilized phase transfer catalyst, wherein the phase transfer catalyst is quaternary ammonium salt or crown ether; the loading capacity of the phase transfer catalyst is 20-40wt%. The invention further provides application of the immobilized phase transfer catalyst in preparation of cumyl peroxyneodecanoate. With adoption of the immobilized phase transfer catalyst provided by the invention, the problems that a homogeneous phase transfer catalyst is difficultly separated from a product and cannot be recycled can be effectively solved; the immobilized phase transfer catalyst can be recycled for fifty times.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and in particular relates to a phase transfer catalyst and its application in the preparation of an initiator. Background technique [0002] With the rapid development of the domestic PVC industry, the variety and demand of initiators for PVC production have increased rapidly. Cumyl peroxyneodecanoate (CNP), as a high-efficiency initiator for PVC production, compared with other types of initiators, has the advantages of less initiator consumption, high initiation efficiency, and high polymerization reaction in the production process of PVC. It has the advantages of uniform heat release and easy control. However, in the existing CNP production process, there are defects such as low production efficiency or difficult separation of the catalyst used after the reaction, resulting in increased production cost. [0003] For example, the Chinese patent document whose publication number is 102532351A d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02C07C407/00C07C409/38
CPCB01J31/0254C07C407/00C07C409/38Y02P20/584
Inventor 席金旭赵长森王会昌牛强
Owner 鄂尔多斯市瀚博科技有限公司
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