• 专利标题:   Preparing epoxidized crosslinked graphene flame-retardant nylon involves adding ethyl orthosilicate to deionized water under stirring to obtain ethyl orthosilicate solution, and mixing with butanol and decabromodiphenyl ethane.
  • 专利号:   CN106893316-A
  • 发明人:   ZHOU Q, CHEN C, ZHAO Y, FU H, ZHAO X, LIU G
  • 专利权人:   ZHOU Q
  • 国际专利分类:   C08K013/06, C08K003/04, C08K003/36, C08K005/03, C08K005/053, C08K009/04, C08L077/02
  • 专利详细信息:   CN106893316-A 27 Jun 2017 C08L-077/02 201765 Pages: 12 Chinese
  • 申请详细信息:   CN106893316-A CN10246624 16 Apr 2017
  • 优先权号:   CN10246624

▎ 摘  要

NOVELTY - Preparing epoxidized crosslinked graphene involves adding 30-40 pts. wt. ethyl orthosilicate to 40-50 times deionized water and mixing under stirring for 2-3 hours to obtain ethyl orthosilicate solution. The 5-6 pts. wt. butanol and 1-2 pts. wt. decabromodiphenyl ethane are added and mixed with the obtained ethyl orthosilicate solution at elevated temperature of 80-85 degrees C under stirring for 20-30 minutes to obtain flame retardant sol. The 0.7-1 pts. wt. bromo-n-butane is added and mixed with 10-16 times anhydrous ethanol under stirring to obtain bromoalcohol dispersion. USE - Method for preparing epoxidized crosslinked graphene flame-retardant nylon (claimed). ADVANTAGE - The method enables to prepare epoxidized crosslinked graphene flame-retardant nylon, which has certain firmness, good barrier property, and effectively improves flame-retardant performance and is cost-effective. DETAILED DESCRIPTION - Preparing epoxidized crosslinked graphene involves adding 30-40 pts. wt. ethyl orthosilicate to 40-50 times deionized water and mixing under stirring for 2-3 hours to obtain ethyl orthosilicate solution. The 5-6 pts. wt. butanol and 1-2 pts. wt. decabromodiphenyl ethane are added and mixed with the obtained ethyl orthosilicate solution at elevated temperature of 80-85 degrees C under stirring for 20-30 minutes to obtain flame retardant sol. The 0.7-1 pts. wt. bromo-n-butane is added and mixed with 10-16 times anhydrous ethanol under stirring to obtain bromoalcohol dispersion. The 6-8 pts. wt. p-hydroxybenzaldehyde is added and mixed with 10-13 times absolute ethanol under stirring then adding 0.2-0.3 pts. wt. metallic sodium with the introduction of nitrogen and allowed to react at 80-90 degrees C for 30-40 minutes. The bromoalcohol dispersion is dropped by maintaining the reaction for 16-20 hours. The ethanol is drop wise added to the reaction system then dried over anhydrous magnesium sulfate to obtain bromobenzaldehyde. The 1-2 pts. wt. tin tetrachloride is added to 3-4 times butanol to obtain mixture solution to obtain tin tetrachloride butanol solution. The bromobenzaldehyde and flame-retardant sol are mixed in reactor by stirring at 55-60 degrees C to obtain mixture solution. The mixture solution is added with 2-4 pts. wt. epichlorohydrin and subjected to insulation treatment for 110-150 minutes to obtain treated mixture solution. The obtained treated mixture solution is added with tin tetrachloride butanol solution at 70-75 degrees C for 40-50 minutes to obtain second mixture. The second mixture is filtered, precipitated, washed and dried at room temperature to obtain epoxidation flame retardant sol. The 2-3 pts. wt. aliphatic amine is added and mixed with 10-17 times absolute ethanol under uniform stirring to obtain aliphatic amine solution. The 15-17 pts. wt. graphene is added and mixed with aliphatic amine solution 60-65 degrees C under stirring for 2 hours to obtain amidated fossil enol liquid. The epoxidized flame-retardant sol is added and mixed with amine fossil enol liquid and subjected to ultrasonic treatment for 10-20 minutes to obtain treated amine fossil enol liquid. The obtained treated amine fossil enol liquid is distilled under vacuum at 60-70 degrees C for 40-50 minutes, where ethanol is removed to obtain epoxidized cross-linked flame retardant graphene. The epoxidized crosslinked flame retardant graphene is mixed with 140-150 pts. wt. nylon, and 4-6 pts. wt. pentaerythritol, under stirring, then feeding into extruder and cooling to obtain the desired product.