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Preparation method of cross-linkable acetal copolymer

A technology of formaldehyde copolymerization and cross-linking polymerization, which is applied in the field of preparation of cross-linkable polyoxymethylene copolymers

Active Publication Date: 2012-07-25
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, there is no report about cross-linked polyoxymethylene

Method used

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  • Preparation method of cross-linkable acetal copolymer
  • Preparation method of cross-linkable acetal copolymer
  • Preparation method of cross-linkable acetal copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add freshly distilled 22.44g TOX, 0.98g DXL and 0.31g GPTMS into a dry nitrogen-filled reaction flask, place in an oil bath at 70°C and stir for 0.5h, mix well and add 4.8μL of initiator HClO 4 , continue to stir, after reacting for 1 h, add 11 μL triethylamine to terminate, wash and filter and dry to obtain 20.55 g of crude product, add 82 mL of DMF solution containing 0.78 g triethanolamine to it for post-treatment at 170 ° C, cool to room temperature, and vacuum-dried the resulting product to obtain 15.23 g of white powdery polymer, to which an appropriate amount of water was added to undergo a cross-linking reaction at 170° C. to form a slightly cross-linked polyoxymethylene copolymer with a gel content of 1%.

Embodiment 2-5

[0033] The polymerization process is the same as in Example 1, except that the ratio of comonomer GPTMS to TOX and DXL is changed. The results are shown in Table 1.

Embodiment 6

[0035] Add freshly distilled 37.97g TOX, 7.81g DXL, 9.96g GPTMS and 19mL cyclohexane into a dry reaction flask filled with nitrogen, place in an oil bath at 70°C and stir for 0.5h, mix well and add 57μL of Initiator HClO 4 , continue to stir, after reacting for 12 hours, add 136 μ L of triethylamine to terminate, wash and filter and dry to obtain 30.55 g of crude product, add 122 mL of DMF solution containing 1.15 g of triethanolamine to it for post-treatment at 170 ° C, and cool to room temperature, and vacuum-dried the resulting product to obtain 10.60 g of white powdery polymer, to which an appropriate amount of water was added to undergo a cross-linking reaction at 170° C. to form a slightly cross-linked polyoxymethylene copolymer with a gel content of 69%.

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Abstract

The invention discloses a preparation method of cross-linkable acetal copolymer. The preparation method is characterized in that: ternary polymerization of (a) trioxymethylene (TOX), (b) dioxolane (DXL) or cyclohexene oxide (CHO) and (c) a triethoxysilane compound with an epoxy group is catalyzed under a water-free and oxygen-free condition in the presence of an initiator BF3 complex or HClO4, wherein the triethoxysilane compound is shown as a formula 1 or 2; R is an alkyl group or aryl group containing 1-18 carbon atoms or a halogen-substituted group containing heteroatoms N, O, S and P, containing no active hydrogen and containing 1-18 carbon atoms; and R2 is an alkyl group containing 1-8 carbon atoms.

Description

technical field [0001] The invention relates to a preparation method of crosslinkable polyoxymethylene copolymer. Background technique [0002] Polyoxymethylene (POM) is an engineering plastic with excellent comprehensive properties. Since the first industrialization of the DuPont company in the United States in 1959, POM has been widely used for its cheap and easy-to-obtain raw materials, convenient processing and molding, good oil resistance, excellent mechanical properties, chemical resistance, low water absorption and good thermal and electrical properties. It is used to replace non-ferrous metals and alloys, and is widely used in automobiles, electronic and electrical industries, various precision machinery, hardware and building materials and other industries. At present, in the entire engineering plastics industry, the annual output of POM is second only to nylon and polycarbonate, becoming one of the top five engineering plastics today. [0003] The existence of he...

Claims

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Application Information

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IPC IPC(8): C08G2/10C08J3/24
Inventor 李化毅贺丽娟张辽云胡友良
Owner INST OF CHEM CHINESE ACAD OF SCI
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