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Polyether end group functionalized polymer prepared by negative ion polymerization technology and preparation method and application thereof

A technology of functionalized polymer and end group, which is applied in the field of polyether end-group functionalized polymer and its preparation, can solve the problem of reducing the end-group functionalization end-capping efficiency, easily producing dimers and multimers, affecting extreme It can improve the processing performance and mechanical properties, low cost and mild preparation conditions.

Active Publication Date: 2020-12-08
DALIAN MARITIME UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Epoxy compounds mainly include ethylene oxide, propylene oxide and their derivatives. At present, there have been studies using negative ion methods to prepare epoxy group-end functionalized polymers, such as East China University of Science and Technology, Beijing University of Chemical Technology, China Petroleum and Natural Gas Co., Ltd., all use epichlorohydrin as the end-capping agent, but there are obvious problems. First, due to the presence of chlorine atoms, it is easy to produce by-products such as dimers and polymers, which reduces the end-group functionalization end-capping agent. Efficiency, affecting the effect of polarized modification
Second, the end-capping efficiency is low, and the reaction conditions are harsh, and it needs to be carried out at an extremely low temperature (-78°C) to obtain high end-capping efficiency

Method used

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  • Polyether end group functionalized polymer prepared by negative ion polymerization technology and preparation method and application thereof
  • Polyether end group functionalized polymer prepared by negative ion polymerization technology and preparation method and application thereof
  • Polyether end group functionalized polymer prepared by negative ion polymerization technology and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0049] The reaction kettle was washed before polymerization, and the inert gas was evacuated. Then, 1500g cyclohexane, 105g butadiene and 45g styrene were introduced in sequence in a 5-liter stainless steel reaction kettle to prepare a solution with a monomer mass concentration of 10%. 1. Add the structure regulator ETE (ethyl tetrahydrofurfuryl ether) according to the molar ratio ETE / n-BuLi=1, start stirring, in a constant temperature water bath at 50°C, according to the design molecular weight of 13×10 4 , add 5.9mmol initiator n-BuLi (n-butyllithium) to initiate polymerization, react for 30 minutes, add DVB (divinylbenzene) according to molar ratio DVB / n-BuLi=2, after coupling reaction for 30min, molar ratio A1(i-Bu) 3 / n-BuLi=10 add catalyst A1(i-Bu) 3 According to the design polyether degree of polymerization = 20, add ethylene oxide and continue to react for 60 minutes at 50°C. Finally, the terminator isopropanol was added to terminate the reaction, the glue solution w...

Embodiment 2

[0056] According to the synthesis method of Example 1, the difference is that only 150g of butadiene monomer is added to form a solution with a monomer mass concentration of 15%, and the structure regulator DTHFP (double tetrahydro furfuryl propane).

[0057] The molecular weight of GPC before and after coupling is 13.1×10 4 and 16.3×10 4 , the molecular weight distributions were 1.04 and 1.10, respectively, and the coupling efficiency was 46.3%. The raw rubber has a moderate viscosity, does not stick to the roller, is easy to mix with additives and fillers, has low heat generation, and is easy to unload, indicating that the prepared end-functionalized polymer has good processability.

Embodiment 3－6

[0059] Prepared according to the method of Example 1, the difference is to change Bd / St (mass ratio), Bd is butadiene, St is styrene, and the mechanical properties of Bd / St and the prepared terminal functionalized polymer composite are shown in Table 4.

[0060] Table 4

[0061]

[0062]

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Abstract

The invention discloses a polyether end group functionalized polymer prepared by a negative ion polymerization technology and a preparation method and application thereof, and belongs to the field ofpreparation of end group functionalized polymers. The method comprises the following steps: firstly, initiating monovinylarene and / or conjugated diene to carry out negative ion polymerization reactionin a hydrocarbon solvent by taking organic lithium as an initiator and a polar organic compound as a regulator to generate an active polymer, secondly, coupling by adopting divinylbenzene to obtain acoupled active polymer, and thirdly, adding an alkyl metal catalyst to obtain the modified active polymer, carrying out an end-capping reaction on the coupled active polymer and an epoxy compound, and carrying out ring-opening polymerization to prepare the polyether end group functionalized polymer. Compared with epoxy chloropropane end capping, the preparation conditions are mild, and the end capping efficiency is high and can reach 90% or above. After coupling, end capping is carried out, and the processability and the mechanical property are improved. The prepared polyether end group functionalized polymer can be applied to the fields of low rolling resistance tires, sound absorption, shock absorption, noise reduction, resin modification and the like.

Description

technical field [0001] The invention belongs to the field of preparation of terminal functionalized polymers, and relates to a polyether terminal functionalized polymer prepared by negative ion polymerization technology, a preparation method and application thereof. Background technique [0002] Functional modification of polymers is one of the important means to achieve high performance and high value. Because the active anion polymerization technology can precisely adjust and control the structural parameters such as the composition, microstructure, sequence distribution, molecular weight and molecular weight distribution of the polymer, especially the unique structure of the end of its active growth chain, it can be combined with functionalized electrophiles. (Also known as end-capping agent) reaction, directly transforming it into various functional groups has become one of the most effective methods for preparing end-functionalized polymers. Generally, the polymers pre...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F236/10C08F212/08
CPCC08F293/00C08F236/10C08F212/08Y02T10/86C08G65/2609C08G2650/24
Inventor 廖明义张春庆王文恒王旭
Owner DALIAN MARITIME UNIVERSITY
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