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Preparation method of copolymer of hydroxybutyl vinyl ether and maleic anhydride

A technology of hydroxybutyl vinyl ether and maleic anhydride is applied in the field of preparation of cross-linked copolymers of vinyl ether and maleic anhydride, can solve problems such as complicated processes, and achieve the effects of simple process, few raw materials and low cost

Inactive Publication Date: 2010-03-03
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is also carried out in two steps, the process is more complicated

Method used

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  • Preparation method of copolymer of hydroxybutyl vinyl ether and maleic anhydride
  • Preparation method of copolymer of hydroxybutyl vinyl ether and maleic anhydride
  • Preparation method of copolymer of hydroxybutyl vinyl ether and maleic anhydride

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Add 367ml (3.75 moles) of ethyl acetate and 135ml (1.25 moles) of cyclohexane into the reactor, mix well, heat to 70°C, then add 122ml (1 mole) of hydroxybutyl vinyl ether and 9.8g (0.1 mol) maleic anhydride, then add 0.5g (0.003 mol) of azobisisobutyronitrile dissolved in 10ml cyclohexane solution at a rate of 0.5ml per minute, react at a constant temperature of 65-70°C for 1 hour, and filter off the clear liquid A crosslinked copolymer of maleic anhydride and hydroxybutyl vinyl ether is obtained. The cross-linked copolymer is a colorless and transparent gel product with no odor, a three-dimensional network cross-linked structure, and a viscosity of 2.12×10 4 centipoise.

[0025] The infrared spectrum of the resulting product is shown in figure 1 Shown, H NMR spectrum and carbon spectrum see figure 2 , image 3 shown. from figure 1 It can be seen in the obtained product that there is no acid anhydride in the alternating copolymer at 1863cm -1 and 1782cm -1 The...

Embodiment 2

[0027] Add 122ml (1.25 moles) of ethyl acetate and 405ml (3.75 moles) of cyclohexane into the reactor, mix well, heat to 60°C, then add 61ml (0.5 moles) of hydroxybutyl vinyl ether and 9.8g (0.1 mol) maleic anhydride, then add 10ml of cyclohexane solution in which 0.61g (0.0015mol) dodecanoyl peroxide has been dissolved at a rate of 0.5ml per minute, react at a constant temperature of 60°C ± 2°C for 3 hours, and filter off The supernatant yielded a cross-linked copolymer of maleic anhydride and hydroxybutyl vinyl ether. The cross-linked copolymer is a colorless, transparent gel product with no odor, a three-dimensional network cross-linked structure, and a viscosity of 1.72×10 4 centipoise.

Embodiment 3

[0029] Add 36.7ml (0.375 moles) of ethyl acetate and 40.5ml (0.375 moles) of cyclohexane into the reactor, mix well, heat to 50°C, then add 13ml (0.1 moles) of hydroxybutyl vinyl ether and 9.8g (0.1 mole) maleic anhydride; then add 10 ml of cyclohexane solution in which 0.083 g (0.0005 mole) of azobisisobutyronitrile has been dissolved at a rate of 0.5 ml per minute, react at a constant temperature of 50 to 55 ° C for 5 hours, filter The supernatant was removed to obtain a cross-linked copolymer of maleic anhydride and hydroxybutyl vinyl ether. The cross-linked copolymer is a colorless, transparent gel product with no odor, a three-dimensional network cross-linked structure, and a viscosity of 1.33×10 4 centipoise.

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Abstract

The invention discloses a preparation method of copolymer of hydroxybutyl vinyl ether and maleic anhydride, which comprises the following steps of: adding the mixed solvent of ethyl acetate and cyclohexane into a reactor; after heating to 50 to 70 DEG C, adding hydroxybutyl vinyl ether and maleic anhydride in sequence, stirring and mixing; then adding cyclohexane liquid containing initiator at a uniform speed ratio in 20 to 40 minutes; and after reacting for 1 to 5 hours at constant temperature, filtering out the clear liquid to obtain crosslinking copolymer of hydroxybutyl vinyl ether and maleic anhydride. The copolymer of hydroxybutyl vinyl ether and maleic anhydride prepared by the preparation method has the advantages of no smell, less material consumption, simple process and low cost,and can expand in a water system to form a transparent gelled product with a netty three-dimensional crosslinking structure.

Description

technical field [0001] The invention relates to a preparation method of a cross-linked copolymer of vinyl ether and maleic anhydride, in particular to a method for preparing a cross-linked copolymer of hydroxy vinyl ether and maleic anhydride. Background technique [0002] Due to its unique linear viscoelastic properties, vinyl ether and maleic anhydride copolymers are widely used in many products such as personal care, agricultural, medical, detergent and cosmetics. However, the product of direct polymerization has low molecular weight and poor application performance, so people have introduced a crosslinking agent to improve the application performance of the copolymer. [0003] In the patent CN97180794.9, it is described: the preparation method of cross-linked maleic anhydride copolymer, which uses polyol compound to cross-link alkyl vinyl ether / maleic anhydride copolymer at 50-90°C to obtain Cross-linked products. Using this method to obtain a cross-linked product requ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F216/14C08F222/06C08F2/06
Inventor 王剑峰田军
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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