Catalytic composite used for ethylene rhodanate resin curing and preparation thereof

A technology of composite catalyst and cyanate ester, which is applied in the field of polymer materials, can solve problems such as the reduction of dielectric properties of resins, and achieve the effects of moderate price, high reactivity and selectivity, and good manufacturability

Inactive Publication Date: 2008-12-17
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But, the dielectric property of the resin that this technical scheme makes also reduces thereupon

Method used

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  • Catalytic composite used for ethylene rhodanate resin curing and preparation thereof
  • Catalytic composite used for ethylene rhodanate resin curing and preparation thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 6.316g of dibutyltin dilaurate and 5.560g of bisphenol A type cyanate, and heat to 60°C under stirring conditions. During this process, a large amount of gas is released. When no more gas is released, the reaction is stopped to obtain Brownish yellow liquid, after cooling to room temperature, organotin compounds can be obtained.

[0020] Weigh 4.080g of cyclopentadiene manganese tricarbonyl and 5.560g of bisphenol A cyanate, dissolve them in methylene chloride at room temperature, and irradiate them under ultraviolet light for 10 minutes to obtain a tan liquid, namely cyclopentadiene Diene manganese tricarbonyl complex solution.

[0021] The organotin compound and cyclopentadiene manganese tricarbonyl complex were mixed at a molar ratio of tin to manganese of 1:10, dissolved in dichloromethane, and stirred for 5 minutes to obtain a composite catalyst.

[0022] Weigh 55.6g (0.2mol) of bisphenol A type cyanate and place it in a beaker, heat it to 90°C and melt it, ...

Embodiment 2

[0025] According to the method of Example 1, an organotin compound and a cyclopentadiene manganese tricarbonyl complex were prepared.

[0026] The organotin compound and cyclopentadiene manganese tricarbonyl complex were mixed at a molar ratio of tin to manganese of 1:15, dissolved in acetone, and stirred for 7 minutes to obtain a composite catalyst.

Embodiment 3

[0028] According to the method of Example 1, an organotin compound and a cyclopentadiene manganese tricarbonyl complex were prepared.

[0029] The organotin compound and cyclopentadiene manganese tricarbonyl complex were mixed at a molar ratio of tin to manganese of 1:20, dissolved in dichloromethane, and stirred for 10 minutes to obtain a composite catalyst.

[0030] Weigh 55.6g (0.2mol) of bisphenol A type cyanate and place it in a beaker, heat it to 90°C and melt it, add 0.002mol of the above-mentioned composite catalyst (calculated by the number of moles of Mn), and stir evenly to obtain uncured Catalyzed resin, its gel time curve see figure 1 Curve c in.

[0031] Pour the uncured catalytic resin into the pre-treated mold, vacuum defoam for 30min, then cure according to the process of 150℃ / 1h+180℃ / 2h, and post-treat at 200℃ for 2h to obtain the cyanide catalyzed by the composite catalyst Ester cured resin, its dielectric properties see figure 2 .

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PUM

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Abstract

The invention relates to a composite catalyst used for hardening cyanate esters and a preparation method thereof and pertains to the technical field of high molecular materials, wherein, the composite catalyst consists of an organic tin compound with a molecular formula of (H9C4)2Sn(NCO-R-OCN)2 and a cyclopentadienyl manganese tricarbonyl composition with a molecular formula of CpMn(CO)(ROCN)2. The preparation method of the composite catalyst is that the organic tin compound and the cyclopentadienyl manganese tricarbonyl composition are blended with the mole ratio of 1:10 to 1:40 and then dissolved in a solution with low toxicity and low boiling point. The composite catalyst which is prepared by the invention and can be used for hardening cyanate esters overcomes defects of the catalyst of single variety and has the advantages of high reaction activity and selectivity, good manufacturability, moderate price, etc.; moreover, the dielectric properties of the catalyzed cyanate resin are obviously better than that of uncatalyzed cyanate resin and the cyanate resin system which adopts only the (H9C4)2Sn(NCO-R-OCN)2 or the CpMn(CO)(ROCN)2 as a catalyst.

Description

technical field [0001] The invention relates to a composite catalyst used for curing reaction of cyanate resin and a preparation method thereof, belonging to the technical field of polymer materials. Background technique [0002] Cyanate resin is a high-performance thermosetting resin matrix developed after the 1970s. Its monomer structure contains two or more cyanate functional groups (-OCN). The cured cyanate has excellent dielectric properties, heat resistance, mechanical properties, low water absorption and good processing properties, and is recognized as the most potential for preparing structure / performance integrated materials in the 21st century base material. [0003] The curing reaction of cyanate resin is characterized by high curing temperature and long curing time. As far as bisphenol A cyanate is concerned, it is cured and heated at 150°C for 48 hours without any catalyst, and the monomer conversion rate is only 48%, higher temperatures and longer times are r...

Claims

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Application Information

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IPC IPC(8): C08G73/06
Inventor 顾嫒娟戴善凯王炳昊顾龙成肖梦雯梁国正袁莉
Owner SUZHOU UNIV
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