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A kind of modified thermosetting resin and preparation method thereof

A thermosetting and resin technology, applied in the field of modified thermosetting resin and its preparation, can solve the problems of not meeting the modification requirements of heat-resistant thermosetting resin, reducing heat resistance, low thermal performance, etc., and achieving good compatibility and interaction , the effect of wide source of raw materials and simple process

Active Publication Date: 2017-09-05
ZHEJIANG LONGXIN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the addition of core-shell microspheres is 5wt%, the impact strength of the modified epoxy resin is 55.8J / m, which is 148% higher than that of the original epoxy resin (Roy P K, Iqbal N, Kumar D, et al. Polysiloxane-based core-shell microspheres for toughening of epoxy resins. Journal of Polymer Research 2014, 21: 1-9), however, the glass transition temperature (Tg) and storage modulus of the modified epoxy resin are both reduced; while the initial decomposition temperature of the core-shell microspheres is only about 280 °C, which cannot Meet the modification requirements of heat-resistant thermosetting resin
[0004]In fact, the research and development of toughening thermosetting resins with core-shell microspheres as a toughening agent has been carried out for many years. The common problem is to reduce the rigidity of the original resin (mold quantity)
For heat-resistant thermosetting resins, there is another serious problem, that is, the reduction of heat resistance
This is mainly because the thermal properties of existing core-shell polymer microspheres are much lower than those of heat-resistant thermosetting resins.

Method used

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  • A kind of modified thermosetting resin and preparation method thereof
  • A kind of modified thermosetting resin and preparation method thereof
  • A kind of modified thermosetting resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Preparation of epoxy polysiloxane microspheres

[0037] Stir 0.50g sodium lauryl sulfate, 0.11g nonylphenol polyoxyethylene ether and 100g deionized water at 100r / min for 5min to obtain a clear and transparent mixed solution A; add 12.02g octamethyl Cyclotetrasiloxane and 5.51g methyltrimethoxysilane were stirred at 300r / min for 10min; ultrasonically stirred for 20min to obtain milky white homogeneous solution B; solution B was heated to 80°C; at a stirring speed of 400r / min, the Add 0.61 p-toluenesulfonic acid to the solution and react for 8 hours; cool down to 60°C, add 1.02g of γ-glycidyl etheroxypropyltrimethoxysilane pre-emulsion dropwise at a rate of 2 drops / second, and then react at 60°C for 2 hours ; At 60° C., add 1.03 g of end-capping agent and react for 1 hour; demulsify, filter, and wash with methanol to obtain epoxy polysiloxane microspheres. The scanning electron micrograph and particle size distribution of this epoxy-based polysiloxane microsphere ar...

Embodiment 2

[0046] Preparation of cured product of modified cyanate resin

[0047] Add 1.21g of polysiloxane-coated polyimide core-shell microspheres and 58.79g of 2,2'-bis(4-cyanophenyl)propane provided in step (2) of Example 1 into the beaker, Stir at 180°C for 2.5h to obtain a prepolymer; pour the prepolymer into a mold, vacuum defoam for 30min, and cure according to the process of 180°C / 2h+200°C / 2h+220°C 2h and 240°C / 4h And heat treatment, the modified cyanate resin is obtained. For its thermal weight loss curve, impact strength, loss factor (tan delt)-temperature change curve and storage modulus-temperature change curve, please refer to the attached Figure 7 , 8 , 9 and 10.

Embodiment 3

[0055] (1) Preparation of polysiloxane-coated polyimide core-shell microspheres

[0056] Add 0.51g sodium lauryl sulfate and 0.12g nonylphenol polyoxyethylene ether to 100g deionized water and stir at 100r / min for 5min to obtain a clear and transparent mixed solution A; Cyclotetrasiloxane, 5.51g methyltriethoxysilane, stirred at 300r / min for 15min; ultrasonically stirred for 20min to obtain milky white homogeneous solution B; solution B was heated to 80°C; at a stirring speed of 450r / min , add 0.61g of p-toluenesulfonic acid, stir and react for 8h, cool down to 60°C, add 1.01g of γ-glycidyl etheroxypropyltrimethoxysilane pre-emulsion dropwise at a rate of 2 drops / second, and then react at 60°C for 2h ; At 60° C., add 1.01 g of end-capping agent and react for 1 h; break the emulsion, filter, and wash with methanol to obtain epoxy polysiloxane microspheres.

[0057] Under argon protection, 8 g of epoxy polysiloxane microspheres were added to a clear and transparent solution con...

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Abstract

The invention discloses a modified thermosetting resin and a preparation method thereof. A modified thermosetting resin can be obtained by uniformly mixing the thermosetting resin and the polyimide core-shell microspheres coated with polysiloxane, and undergoing curing and post-treatment processes. The polysiloxane-coated polyimide core-shell microspheres of the present invention have outstanding thermal stability, and have -NH2 on the surface. Compared with the existing thermosetting resin, the modified thermosetting resin prepared by the invention has high impact strength, storage modulus and outstanding heat resistance. At the same time, the preparation method of the modified thermosetting resin provided by the invention also has the advantages of wide source of raw materials, simple process and the like.

Description

technical field [0001] The invention relates to a thermosetting resin and a preparation method thereof, in particular to a modified thermosetting resin and a preparation method thereof. Background technique [0002] The rapidly developing modern industry has a surge in demand for polymers with outstanding heat resistance (high glass transition temperature and thermal stability). However, brittleness has always been the main deficiency of thermosetting resins. So far, people have found a variety of toughening methods for thermosetting resins, and the methods with significant toughening effects are mainly rubber toughening, blending / copolymerization with engineering thermoplastic resins, etc. Among them, the biggest advantage of rubber toughening is that the toughening effect is remarkable, but it often leads to a substantial decrease in heat resistance. This is more prominent in the toughening of heat-resistant thermosetting resins. However, the use of engineering thermopl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/06C08G73/10C08G59/00C08G77/14C08L63/00C08L79/04C08L79/08C08L83/06
Inventor 顾嫒娟董鑫怡梁国正袁莉
Owner ZHEJIANG LONGXIN CHEM CO LTD
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