Method for preparing boron phenolic/in-situ nano hybrid compound resin

A boron phenolic resin and hybrid composite technology are applied in the field of preparation of boron phenolic/in-situ nano-hybrid composite resin, which can solve problems such as the inability to ensure uniform dispersion of nanoparticles, and achieve hydrolysis resistance stability, easy operation and control. , the effect of good thermal stability

Inactive Publication Date: 2008-05-14
HEBEI UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In boron phenolic resin / nano-SiO 2 In the research of hybrid composite resin, Qiu Jun and Wang Guojianli (CN1844179A) dispersed nano-SiO in the synthesis or in the solid 2 The method prepared phenol / boric acid / paraformaldehyde type boron phenolic / nano-SiO 2 Composite resins, but this blending method uses the direct addition of SiO to the reaction solution 2 , does not guarantee uniform dispersion of nanoparticles

Method used

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  • Method for preparing boron phenolic/in-situ nano hybrid compound resin
  • Method for preparing boron phenolic/in-situ nano hybrid compound resin

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Experimental program
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Effect test

Embodiment 1

[0034] Embodiment 1: Preparation of boron-nitrogen coordination boron phenolic resin / nano-montmorillonite composite resin

[0035](1) The synthesis of boron-nitrogen coordination compound is added in the reaction flask according to the molar ratio of boric acid and phenol 1:2, and an appropriate amount of 30-50mL toluene is added, the temperature is raised to reflux, and the esterification reaction water is continuously separated by the oil-water separator, At the same time, the reaction temperature is gradually increased to accelerate the esterification reaction, and the reaction temperature is controlled at 110-160° C. until the theoretical dehydration amount is reached, and the reaction is terminated. After the temperature of the reaction system drops below 100°C, add 1 mole of aminoethanol to continue the reaction until complete to obtain a purple-red coordination type triphenyl borate monomer.

[0036] (2) Add paraformaldehyde or paraformaldehyde according to the molar ra...

Embodiment 2

[0040] Embodiment 2: boron nitrogen coordination boron phenolic resin / nanometer SiO 2 Preparation of composite resin

[0041] (1) same as embodiment 1;

[0042] (2) Trimeric or paraformaldehyde, 0.01 oxalic acid or NaOH of 1.2-1.4 times molar weight of phenol molar weight are added in the second stage of reaction, while adding tetramethoxysilane or tetramethoxysilane of 6-30% of phenol weight Ethoxysilane, react at 80-140°C for 1-2 hours. In the later stage of the reaction, water, solvent toluene or xylene and hydrolysis product methanol or ethanol are removed under reduced pressure. As the dehydration reaction under reduced pressure proceeds, the viscosity of the system continues to increase, and the reaction can be accelerated by appropriately increasing the reaction temperature (controlled below 140°C) to reduce the viscosity of the system until the polyoxymethylene is fully reacted, and purple-yellow solid boron nitrogen can be obtained Coordinated boron phenolic / nano-S...

Embodiment 3

[0044] Embodiment 3: Formaldehyde aqueous solution method prepares boron phenolic / nanometer montmorillonite composite resin

[0045] (1) Add phenol and 37% formaldehyde aqueous solution into the reaction flask according to the molar ratio of phenol and formaldehyde 1: 1.2, and add NaOH or Ba(OH) of 0.02-.0.05 molar amount of phenol at the same time 2 Solution, heated up and reacted at 60-70°C for 60 minutes, dehydrated under reduced pressure to obtain salicyl alcohol;

[0046] (2) Adding boric acid at a molar ratio of phenol to boric acid 3:0.5-1.0 and simultaneously heating up the reaction, controlling the reaction temperature at 100-105° C.;

[0047] (3) After the above reaction for 30-60 minutes, add 3-15% organic montmorillonite based on the weight of phenol, and continue to react under this condition for 30-60 minutes, dehydrating under reduced pressure. Control the reaction temperature between 105-115°C while avoiding gelation. The end point of the reaction can be trac...

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Abstract

The invention relates to a preparation method of boron phenolic / in-situ nano-hybrid composite resin, wherein the boron content in boron phenolic is calculated as 3.0:0.3-1.0 according to the molar ratio of phenolic hydroxyl group to boric acid, and is characterized in that: in the preparation of boron phenolic After 30-60 minutes of resin resinization reaction, add organic montmorillonite or tetramethoxysilane with 5-30% phenol weight of the reaction raw material to the solution, and react at a temperature of 105-130°C for 40-90 minutes. The gelation time is 60-120s / 200°C to control the reaction end point, and the reaction solvent is removed under reduced pressure to obtain boron phenolic / in-situ intercalation or in-situ generated nano-hybrid composite solid resin. The present invention uses in-situ intercalation or in-situ generation to prepare nano-composite materials, which ensures the dispersion uniformity of inorganic nano-materials in resins; compared with non-hybrid composite resins, the obtained resins have better thermal stability and high temperature Residual rate, mechanical properties and stability against hydrolysis; the preparation process is simple, convenient, easy to operate and control.

Description

technical field [0001] The invention relates to a preparation method of boron phenolic / in-situ nano-hybrid composite resin, which belongs to the technical field of chemical synthesis. Background technique [0002] Boron phenolic resin is a modified phenolic resin in which boron is introduced into ordinary phenolic resin, and has a wide range of uses in aerospace and other fields. With the development and application of nanomaterials, the modification of boron phenolic with inorganic nanomaterials has become an important means of polymer material modification by using itself and the nano-solid effect formed by it to make it have a series of excellent properties. In boron phenolic resin / nano-SiO 2 In the research of hybrid composite resin, Qiu Jun and Wang Guojianli (CN1844179A) dispersed nano-SiO in the synthesis or in the solid 2 The method prepared phenol / boric acid / paraformaldehyde type boron phenolic / nano-SiO 2 Composite resins, but this blending method uses the direct...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/10C08K9/04C08G8/10C08K3/36
Inventor 高俊刚刘彦方夏丽娅蒋超杰翟丁苏小辉
Owner HEBEI UNIVERSITY
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