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Intercalator and preparation method thereof

An intercalating agent and amine compound technology, applied in the chemical field, can solve the problems of increasing the interlayer spacing of montmorillonite, unable to help montmorillonite peel off, and unable to promote interlayer reaction, etc.

Active Publication Date: 2012-08-08
WUXI ACRYL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Analysis of existing patents shows that most systems use long-chain aliphatic ammonium salts as organic modifiers to increase the interlayer distance of montmorillonite and help epoxy resin and curing agent enter the interlayer reaction. This type of modifier It does not promote the interlayer reaction, so it cannot make the epoxy and curing agent molecules entering the interlayer react before the whole system, thus helping to obtain the exfoliated montmorillonite-epoxy composite material. Therefore, using this type of intercalation In the preparation process, high temperature or strong shear force is often required to obtain exfoliated composite materials, which increases the complexity of the process and the instability of material properties.
"US5801216" selects a modifier containing active groups, but its function is to bond the montmorillonite into the crosslinking system, and it cannot help the stripping of the montmorillonite

Method used

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  • Intercalator and preparation method thereof
  • Intercalator and preparation method thereof
  • Intercalator and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035]Example 1, 232g of hexamethylenediamine and 169.2g of phenol were mixed in a reactor, the temperature was controlled at 50°C, and 146g of formaldehyde with a concentration of 37% was added dropwise at a stirring speed of 200 rpm, within 2 hours The dropwise addition was completed; after the dropwise addition was completed, the reaction was continued for 1 hour; the temperature of the reactor was raised to 95°C, and the reaction was carried out for 4 hours; The molecular structural formula of the agent is:

[0036]

[0037] The obtained intercalation agent is used to prepare organically modified montmorillonite: the obtained intercalation agent is mixed with deionized water according to the ratio of 1:10 by weight, and a hydrochloric acid solution with a concentration of 5mol / L is added dropwise to pH The value is between 6 and 7, and the intercalation agent salt solution is obtained;

[0038] Disperse 20 g of montmorillonite in 500 g of ionized water, stir for 30 min...

Embodiment 2

[0040] Example 2, add 460g of amino-terminated polyether D-230 into the reactor, add 146g of formaldehyde dropwise at a stirring speed of 200 rpm, control the temperature not to exceed 45°C, and complete the dropwise addition within 1 hour; After the addition was completed, the reaction was continued for 1 hour; 169.2 g of phenol was added to the reactor, the temperature was raised to 60° C., and the reaction was carried out for 2 hours; the temperature was raised to 95° C., and the reaction was carried out for 4 hours; 638.5g of intercalation agent, the obtained intercalation agent structure is:

[0041]

Embodiment 3

[0042] Example 3, 272g of m-xylylenediamine was added to the reactor, 146g of formaldehyde was added dropwise at a stirring speed of 200 rpm, the temperature was controlled not to exceed 45°C, and the dropwise addition was completed within 2 hours; the dropwise addition was completed Then, continue to react for 1 hour; add phenol into the reactor, heat up to 60°C, and react for 2 hours; heat up to 95°C, react for 4 hours; heat up to 120°C, react for 2 hours, effluent 119.3g, and obtain 458g agent, the obtained intercalator structure is:

[0043]

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Abstract

The invention relates to a preparation method of an intercalator. The preparation method is characterized by comprising the following steps of: adding an amine compound into a reactor, dripping formaldehyde at a stirring speed of 20-500 turns / min and a controlled temperature of 25-45 DEG C and finishing the dripping within 0.5-4 h; continuously reacting for 0.5-2 h after the dripping is finished;adding a phenolic compound into the reactor, increasing the temperature to 50-60 DEG C and reacting for 0.5-2 h; increasing the temperature to 80-100 DEG C and reacting for 2-6 h; and increasing the temperature to 120-150 DEG C and reacting for 2-6 h to evaporate water content and obtain the intercalator. Compared with a traditional intercalator, the intercalator structure provided by the invention contains phenyl or phenyl sulfide for intercalating montmorillonite layers to not only increase the distance among the montmorillonite layers and the possibility for epoxy and a curing agent to enter the interlamination, but also effectively promote the reaction activity of the epoxy groups and the amino of the interlamination and preferentially carry out the interlamination reaction to the whole system so as to stimulate the interlamination stripping of the montmorillonite.

Description

technical field [0001] The invention relates to an intercalation agent, in particular to an intercalation agent for preparing organic montmorillonite and a preparation method thereof, belonging to the field of chemistry. Background technique [0002] Epoxy resin is a kind of thermosetting polymer synthetic material with excellent properties. It is widely used in the fields of composite materials, electrical insulation materials, coatings and adhesives because of its excellent mechanical properties, electrical properties and adhesive properties. The traditional epoxy resin curing system is brittle and poor in impact resistance and fatigue resistance, which largely limits its application fields. In recent years, with the development of wind energy and large aircraft industry, large-scale composite materials such as megawatt wind power blades and fuselages have put forward higher requirements for the mechanical properties of materials. The final strength, toughness and fatigue...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/04C08K3/34C08L63/00C07C215/50C07C213/02C07C217/08
Inventor 张文泉王俊卿朱学军尤卫民
Owner WUXI ACRYL TECH