Synthesis And Phosphorylation Research Of Phenolic Derivatives

In this paper, the synthesis method of 2,2’- methylene- bis(4-t-butylphenol) and 2,2’-methylene- bis(6-t-butylphenol) was researched in detail. 2,2’-methylene-bis(4-tertbutylphenol) was synthesized through Inverse Friedel-Crafts alkylation with 2,2’-methylene-bis(4,6-ditertbutylphenol) as a raw material. The synthesized product was analysis and determination by means of FTIR, NMR, DSC, TGA,WXRD,MS,etc. The results showed: The yield is 80%. The melting temperature of product were 155 ℃. MS results showed that the relative molecular mass is 312g/mol. 2,2’-methylenebis(6-t-butylphenol) was synthesized with 2-t-butyl phenol and paraformaldehyde as a raw material and xylene as solvent.The reaction was operated under high temperature and pressure. The synthesized product was analysis and determination by means of FTIR, NMR, DSC, TGA,WXRD,MS,etc. The results showed: The yield is 96%. The melting temperature of product were 108.3 ℃. MS results showed that the relative molecular mass is 312g/mol.2,2’-Methylene-bis(4-tert-butylphenyl)Phosphate Chloride was synthesized through catalyst triethylamine with 2,2’-methylene-bis(4-tertbutylphenol) and phosphornsoxychloride. 2,2’- methylene- bis(4-t-butylphenyl) sodium phosphate was prepared through hydrolysis and salt formation with 2,2’-Methylene-bis(4-tert-butylphenyl)Phosphate C hloride as a raw material.2,2’- methylene- bis(6-t-butylphenyl) sodium phosphate was synthesized through the same reaction with 2,2’-methylene-bis(4-tertbutylphenol) as a raw material. The above product was analysis and determination by means of FTIR, NMR, DSC, TGA,WXRD,MS,etc.Compared with nucleating agent NA-11 of ASAHI DENKA’s production, the differences of nucleated effectiveness with ortho-substituted or para-substituted groups of Aromatic Heterocyclic phosphate Salts(sodium 2,2’- methylenebis(4-t-butylphenyl) phosphate and sodium 2,2’-methylenebis(6-t-butylphenyl) phosphate) resulted in were studied. The results showed:(1)The addition of nucleating agent is 2‰.Compared with nucleating agent NA-11, the crystallization peak temperature, tensile strength, flexural strength and flexural modulus, vicat softening temperature of sodium 2,2’- methylenebis(4-t-butylphenyl) phosphate reduced 8.45 ℃, 0.9MPa, 3.7MPa, 168.4MPa and 5.4 ℃ respectively.(2)The addition of nucleating agent is 2‰. Compared with nucleating agent NA-11, the results of DSC show that when sodium 2,2’- methylenebis(6-t-butylphenyl) phosphate) was added, there were two crystallization peak of 117℃ and 129℃;the tensile strength, flexural strength and flexural modulus, vicat softening temperature of sodium 2,2’-methylenebis(6-t-butylphenyl) phosphate reduced 2.3MPa, 3.1MPa, 335 MPa and 8.6℃ respectively.