In-situ preparation method of nano cellulose surface grafted nylon 6 composite material

A nano-cellulose, in-situ preparation technology is applied in the field of in-situ preparation of nano-cellulose surface grafted nylon 6 composite materials, which can solve the problems of insufficient interface bonding and uneven dispersion of nano-materials, so as to reduce polymerization inhibition, The effect of improving overall performance and avoiding insufficient heat resistance

Inactive Publication Date: 2021-10-22
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The purpose of the present invention is to provide an in-situ preparation method of nano-cellulose grafted nylon 6 composite material to solve the problems of uneven dispersion of nano-materials in the polymer matrix and insufficient interfacial bonding

Method used

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  • In-situ preparation method of nano cellulose surface grafted nylon 6 composite material

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Experimental program
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Embodiment 1

[0041] Weigh 10.00g of cellulose nanocrystals (CNC) and vacuumize at 120°C to remove water for 48h, and after cooling in N 2 Add 100mL of toluene under the atmosphere, sonicate for 30min, then add 30.0mL of triethylamine and 27.0mL of 2,4-toluene diisocyanate successively, stir and heat at 35°C for 24h, centrifuge after the reaction to obtain a precipitate. Wash with toluene to remove unreacted triethylamine and 2,4-toluene diisocyanate, centrifuge to discard the supernatant, and dry the precipitate in a vacuum oven at 30°C for 12 hours; then, the dried isocyanated Cellulose nanocrystal powder is placed in the flask and evacuated for 10min, under N 2 Add 500mL of toluene under the atmosphere, ultrasonic for 0.5h; weigh 95.60g of caprolactam, vacuumize and remove water at 110°C for 0.5h, cool it under N 2 Add 500mL of toluene at low temperature and stir until completely dissolved; slowly add the toluene solution of caprolactam into the toluene mixture of isocyanated cellulose ...

Embodiment 2

[0044] Weigh 10.00g of microcrystalline cellulose nanocrystals (MCC) and vacuumize at 120°C to remove water for 48h, and after cooling in N 2 Add 100mL of toluene under the atmosphere, sonicate for 30min, then add 60.0mL of triethylamine and 54.0mL of 2,4-toluene diisocyanate in sequence, stir and heat at 45°C for 24h, centrifuge after reaction to obtain a precipitate. Wash with toluene to remove unreacted triethylamine and 2,4-toluene diisocyanate, centrifuge to discard the supernatant and dry in a vacuum oven at 30°C for 12 hours; then, the dried isocyanated fibers Prime nanocrystalline powder is placed in the flask and evacuated for 10min, under N 2 Add 900mL of toluene under the atmosphere, ultrasonic for 0.5h; weigh 85.60g of caprolactam, vacuumize and remove water at 110°C for 0.5h, cool it under N 2 Add 900mL toluene at low temperature and stir until completely dissolved; slowly add the toluene solution of caprolactam into the toluene mixture of isocyanated cellulose n...

Embodiment 3

[0047] Weigh 10.00g of cellulose nanofibers (CNF) and vacuumize at 120°C to remove water for 48h, and after cooling in N 2 Add 500mL of toluene under the atmosphere, sonicate for 30min, then add 30.0mL of triethylamine and 27.0mL of 2,4-toluene diisocyanate in sequence, stir and heat at 45°C for 24h, centrifuge after reaction to obtain a precipitate. Wash with toluene to remove unreacted triethylamine and 2,4-toluene diisocyanate, centrifuge to discard the supernatant and dry in a vacuum oven at 30°C for 12 hours; then, the dried isocyanated fibers Prime nanocrystalline powder is placed in the flask and evacuated for 10min, under N 2 Add 50mL of toluene under the atmosphere, sonicate for 0.5h; weigh 42.80g caprolactam, vacuumize and remove water at 110°C for 0.5h, cool it under N 2 Add 200mL of toluene at low temperature and stir until completely dissolved; slowly add the toluene solution of caprolactam into the toluene mixture of isocyanated cellulose nanocrystals, raise the...

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Abstract

The invention discloses an in-situ preparation method of a nano cellulose surface grafted nylon 6 composite material, and relates to the technical field of polymer processing. Cellulose nanocrystal grafted caprolactam with different proportions and different grafting rates is used as an activator, and a low-activity initiator is used to initiate in-situ ring opening polymerization of caprolactam at a low temperature. The nano cellulose grafted nylon 6 composite material is prepared by the one-step method. The polymerization process can be completed in a short time, and meanwhile, high conversion rate and crystallinity can be achieved. According to the invention, the in-situ polymerization method is adopted, so that the nano cellulose is dispersed more uniformly in the resin, and the interface performance of the composite material is improved through a chemical grafting mode. The mechanical property and the heat resistance of the material are remarkably improved, and the process is simple, high in efficiency and wide in application prospect.

Description

technical field [0001] The invention relates to the technical field of polymer processing, in particular to an in-situ preparation method of a nano-cellulose surface-grafted nylon 6 composite material. Background technique [0002] As an engineering plastic widely used in industrial and daily life products, nylon 6 has the advantages of high strength, high toughness, wear resistance, self-lubrication, chemical resistance and strong chemical solvent resistance. However, nylon 6 has poor impact resistance at low temperature and dry state, insufficient rigidity and heat resistance under strong external force and heating conditions, and poor dimensional stability of products. These factors limit its partial application. In order to overcome the above shortcomings, it is usually modified by blending filling, block and grafting methods in practical applications. Among them, the use of nanoparticle filling is an important way to achieve high performance and functionalization of po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/16C08L77/02C08L1/04
CPCC08G69/16C08L77/02C08L1/04
Inventor 阚泽史豪孙阿彬张晓潭
Owner QINGDAO UNIV OF SCI & TECH
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