Double-modification polyacrylonitrile fiber metal complex catalyst and preparation method thereof
A technology of polyacrylonitrile fibers and metal complexes, applied in the direction of organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of poor physical and mechanical properties and catalytic activity Problems such as too fast decline and low stability in use have achieved the effects of easy operation, easy industrial promotion, and many times of repeated use
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Embodiment 1
[0040] 1. Pretreatment of polyacrylonitrile fiber: Wash the polyacrylonitrile fiber yarn with nonionic surfactant JFC aqueous solution containing volume concentration of 2.0g / L for 30 minutes, take it out, wash it twice with water, and dry it for later use.
[0041] 2. Hydrazine hydrate mixed modification reaction of polyacrylonitrile fiber: accurately weigh 10 grams of the pretreated polyacrylonitrile fiber, and immerse it in 250 milliliters of hydrazine hydrate with a volume concentration of 80 g / L and a volume concentration of 5 g / L In the aqueous solution of hydroxylamine hydrochloride, the ratio of polyacrylonitrile fiber weight (grams) to the volume (milliliters) of the aqueous solution is 1:25; then react at 93°C for 4 hours under stirring conditions, and after the reaction, the obtained brown mixture is modified The polyacrylonitrile fiber (M-PAN-1 for short) was taken out, washed 5 times with distilled water, weighed after drying, and its weight gain rate was 32.54%; ...
Embodiment 2
[0048] 1, 4 and 5 step processes are respectively the same as 1, 4 and 5 step processes in Example 1.
[0049] 2. Hydrazine hydrate mixed modification reaction of polyacrylonitrile fibers: accurately weigh 10 grams of the pretreated polyacrylonitrile fibers, and immerse them in hydrazine hydrate and 12g / L hydroxylamine hydrochloride aqueous solution whose volume concentration is respectively 65g / L to make the polyacrylonitrile fibers The ratio of the weight of acrylonitrile fiber (grams) to the volume (milliliters) of the aqueous solution is 1:25; then react for 3 hours at 82°C under stirring conditions, and the obtained brown mixed modified polyacrylonitrile fiber (abbreviated as M- PAN-2) was taken out, washed 5 times with distilled water, weighed after drying, and its weight gain rate was 25.86%;
[0050] 3. Sodium hydroxide partial hydrolysis reaction: first prepare 378 milliliters of molar concentration ratios and be the mixed solution of ethanol and water of 1: 5, and ad...
Embodiment 3
[0053] 1, 4 and 5 step processes are respectively the same as 1, 4 and 5 step processes in Example 1.
[0054] 2. Hydrazine hydrate mixed modification reaction of polyacrylonitrile fibers: accurately weigh 10 grams of the pretreated polyacrylonitrile fibers, and immerse them in hydrazine hydrate with a volume concentration of 40 g / L and in an aqueous solution of hydroxylamine hydrochloride with a volume concentration of 20 g / L , make the ratio of polyacrylonitrile fiber weight (gram) and the volume (milliliter) of aqueous solution be 1: 25; Then react 1.5 hours under 75 ℃ and stirring condition, the brown mixed modified polyacrylonitrile fiber ( Abbreviated as M-PAN-3) was taken out, washed 5 times with distilled water, dried and weighed, the weight gain rate was 18.47%;
[0055] 3. Sodium hydroxide partial hydrolysis reaction: first prepare 357 milliliters of molar concentration ratios and be the mixed solution of ethanol and water of 1: 5, and add the sodium hydroxide of 35....
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