Polyhedral oligomeric silsesquioxane phosphate nucleating agent as well as preparation method and application thereof
A silsesquioxane and siloxane technology, which is applied in the field of cage-type silsesquioxane phosphate nucleating agents and their preparation, can solve problems such as limitations, and achieve improved crystalline structure and increased crystallization temperature. , the effect of improving the nucleation efficiency
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Embodiment 1
[0044] A kind of preparation method of cage type silsesquioxane phosphate nucleating agent is as follows: heptameric isobutyl monoglycidyl cage type silsesquioxane (POSS) (0.01mol, 13.37g) (structure The above-mentioned cage silsesquioxane should be 2 in the structural formula 1-5, wherein the substituent R 1-7 Both are isobutyl, R 8Glycidyl, purchased from American hybrid plastics company, item number is EP0409) and 2,2'-methylene-bis-(4,6-di-tert-butylphenyl)phosphoryl chloride (0.01mol, 4.82g) ( The structure is a phosphate ester structure shown in formula I, wherein the substituent R 1-4 Respectively CH 2 , tert-butyl, tert-butyl, Cl) were mixed in 100mL THF solution, the mixture was heated to reflux for 3h under vigorous stirring, the solvent was removed by distillation under reduced pressure, and the cage-type silsesquioxane phosphate compounds were obtained by washing with water. nuclear agent.
[0045] The structure of 2,2'-methylene-bis-(4,6-di-tert-butylphenyl) p...
Embodiment 2
[0056] A kind of preparation method of cage type silsesquioxane phosphate nucleating agent is as follows: Octalanilino cage type silsesquioxane (POSS) (5mmol, 5.765g) (structure is above-mentioned cage type silsesquioxane Siloxane should be 2 in the structural formula 1-5, wherein the substituent R 1-8 Both are anilino, purchased from American hybrid plastics company, item number is AM0280) and 2,2'-methylene-bis-(4,6-di-tert-butylphenyl) phosphate (40mmol, 19.28g) (structure is the phosphate ester structure shown in formula I, wherein the substituent R 1-4 Respectively CH 2 , tert-butyl, tert-butyl, OH) were mixed in 100mL methanol solution, the mixture was heated to reflux for 3h under vigorous stirring, the solvent was removed by distillation under reduced pressure, and the cage-type silsesquioxane phosphate compound was obtained by washing with water. nuclear agent.
[0057] The structure of 2,2'-methylene-bis-(4,6-di-tert-butylphenyl)phosphate is as follows:
[0058] ...
Embodiment 3
[0064] A kind of preparation method of cage type silsesquioxane phosphate nucleating agent is as follows: heptameric isobutyl monoamino cage type silsesquioxane (POSS) (0.01mol, 8.74g) (structure is above-mentioned Cage silsesquioxane should be 2 in the structural formula 1-5, wherein the substituent R 1-7 is isobutyl, R 8 for -(CH 2 ) 3 -NH 2 , purchased from American hybrid plastics company, the article number is AM0265) and 2,2'-methylene-bis-(4,6-di-tert-butylphenyl) phosphate (0.01mol, 4.82g) (the structure is the above-mentioned phosphoric acid 1 in the ester structural formula 1-2, wherein the substituent R 1-4 Respectively CH 2 , tert-butyl, tert-butyl, OH) were mixed in 100mL methanol solution, the mixture was heated to reflux for 3h under vigorous stirring, the solvent was removed by distillation under reduced pressure, and the cage-type silsesquioxane phosphate compound was obtained by washing with water. nuclear agent.
[0065] A kind of preparation method o...
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