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Preparation method of polyamide polyamine intercalated layered silicate composite material

A technology of polyamide polyamine and layered silicate is applied in the field of modified polyamide polyamine, which can solve the problems of low rigidity, low heat resistance and poor wear resistance of polyamide polyamine, and achieve the effect of improving strength

Inactive Publication Date: 2017-07-28
湖南省达琪新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on this, it is necessary to provide a method for preparing a polyamide polyamine intercalated layered silicate composite material for the problems in the background technology. The polyamide polyamine intercalated layered silicate composite material prepared by the preparation method is The material not only solves the shortcomings of polyamide polyamine such as low heat resistance, low rigidity, and poor wear resistance, but also strengthens its advantages such as good adhesion and toughness.

Method used

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Examples

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preparation example Construction

[0027] A preparation method of polyamide polyamine intercalated layered silicate composite material, comprising the following steps:

[0028] S110. Mix organic carboxylic acid, polyamine, deionized water, coupling agent, defoamer and layered silicate compound evenly, raise the temperature to 110°C~130°C in a nitrogen atmosphere, maintain the pressure ≤0.3MPa, and stir 1 to 3 hours, slowly release the pressure to normal pressure and then reflux for 1 to 3 hours, then raise the temperature to 130°C to 150°C, stir for 1 to 2 hours, and dehydrate to obtain a pre-intercalation mixture.

[0029] Wherein, the mass ratio relation between each raw material is as follows:

[0030] 55.5~96.3 parts of organic carboxylic acid and polyamine;

[0031] 0.5~5 parts of deionized water;

[0032] 0.1~3.5 parts of coupling agent;

[0033] Defoamer 0.1~1.0 parts;

[0034] Layered silicate compound 3~35 parts.

[0035] Preferably, the mass ratio relationship between the above-mentioned raw mate...

Embodiment 1

[0059] 560g (1mol) vegetable oleic acid dimer, 13.2g (0.1mol) glutaric acid, 7g (0.025mol) linoleic acid, 292g (2mol) triethylenetetramine, 12.9g (0.1mol) N-aminoethyl Mix piperazine, 30g deionized water, 8g aminopropyltrimethoxysilane, 4g tributyl phosphate and 80g 1250 mesh montmorillonite evenly, raise the temperature to 120°C in a nitrogen atmosphere, maintain the pressure at 0.2MPa and stir for 1 hour, slowly release Press down to normal pressure and reflux for 1 hour, then raise the temperature to 140°C and stir for 1.5 hours, dehydrate, then raise the temperature to 205°C, maintain 0.5MPa for 3 hours, slowly release the pressure to normal pressure, dehydrate and continue the reaction for 2 hours, and depressurize to Under vacuum conditions, the unreacted polyamine and the water produced by the reaction are removed, the temperature is lowered to below 60° C., and the mixture is stirred for 2.5 hours to obtain a polyamide polyamine intercalated layered silicate composite m...

Embodiment 2

[0062] 420g (0.75mol) vegetable oleic acid dimer, 66g (0.5mol) glutaric acid, 3.6g (0.025mol) 2-ethylhexanoic acid, 292g (2mol) triethylenetetramine, 12.9g (0.1mol) N -Aminoethylpiperazine, 30g deionized water, 10g aminopropyltriethoxysilane, 6g tributyl phosphate and 90g 1250 mesh montmorillonite were mixed evenly, heated to 130°C in a nitrogen atmosphere, and kept stirring at a pressure of 0.3MPa 1 hour, slowly release the pressure to normal pressure and then reflux for 1 hour, then raise the temperature to 150°C and stir for 1.5 hours, dehydrate, then raise the temperature to 200°C, maintain 0.5MPa for 3 hours, slowly release the pressure to normal pressure, then dehydrate and continue the reaction 2 Hours, depressurize to vacuum conditions, remove unreacted polyamines and water produced by the reaction, then lower the temperature to below 60°C, and stir for 2.5 hours to obtain a polyamide polyamine intercalated layered silicate composite material.

[0063] Samples were cur...

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Abstract

The invention provides a preparation method of a polyamide polyamine intercalated layered silicate composite material. The preparation method comprises the following steps: uniformly mixing organic carboxylic acid, polyamine, deionized water, a coupling agent, a defoaming agent and a layered silicate compound, heating to 110 to 130 DEG C in a nitrogen atmosphere, retaining the pressure to be less than or equal to 0.3 MPa, stirring for 1 to 3 hours, slowly relieving the pressure to normal pressure, then performing reflux for 1 to 3 hours, heating to 130 to 150 DEG C again, stirring for 1 to 2 hours, performing dewatering, and obtaining the polyamide polyamine intercalated layered silicate composite material in combination with in-situ polymerization intercalation and delamination and reassembling intercalation. The polyamide polyamine intercalated layered silicate composite material is used for curing epoxy resin; the thermal deformation temperature of a cured product is increased by 30 DEG C or above; and the toughness, the adhesiveness, the wear resistance and the strength are all further improved.

Description

technical field [0001] The invention relates to a modified polyamide polyamine, in particular to a polyamide polyamine intercalated layered silicate composite material. Background technique [0002] Polyamide polyamine is widely used in the curing of epoxy resin because of its good adhesion and good toughness of the cured product, but the heat resistance of the cured product is low (heat distortion temperature <80°C), Disadvantages such as low rigidity and poor wear resistance also limit its application range. [0003] The traditional method to solve the shortcomings of polyamide polyamine is to improve its performance by adjusting the formula, such as adding some special epoxy resin or adding some special performance curing agent. However, it is difficult to have a formula that can maintain its good adhesion and toughness, while improving its heat resistance, rigidity, wear resistance, etc., and some even increase toxicity. Contents of the invention [0004] Based on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/34C08G69/28C08K3/34C08L77/06
CPCC08G69/34C08G69/28C08K3/346C08L77/06
Inventor 谭国权
Owner 湖南省达琪新材料有限公司
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