Formaldehyde condensate of alkylphenol ethoxylate esters and preparation method of formaldehyde condensate
A technology of alkylphenol polyoxyethylene ether and formaldehyde dimer is applied in the preparation of organic compounds, ether preparation, carboxylate preparation and other directions, and can solve the problems of long production cycle, long settling time, unfavorable industrial production and the like, Achieve the effect of low production cost, low dosage, and easy industrialized continuous production
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[0032] One aspect of the embodiments of the present invention provides a method for preparing a formaldehyde polycondensate of an alkylphenol polyoxyethylene ether ester, comprising the following steps:
[0033] S1: Using substituted alkylphenols and linear polymers of formaldehyde to undergo polycondensation reaction under the action of acidic or basic catalysts to obtain formaldehyde dimers or trimers of alkylphenols;
[0034] S2: Use the formaldehyde dimer or trimer of the alkylphenol and the alkylene oxide to undergo a ring-opening polyaddition reaction under the action of a basic catalyst to obtain an alkylphenol polyvinyl ether formaldehyde dimer or trimer condensation polymer;
[0035] S3: Utilize the alkylphenol polyvinyl ether dimer polycondensate or trimer polycondensate and acid anhydride to undergo esterification reaction under the action of an acid catalyst or a basic catalyst to obtain formaldehyde polycondensation of an alkylphenol polyoxyethylene ether esterifi...
Embodiment 1
[0054] Embodiment 1: the preparation of 2,6-dimethylol-4-nonylphenol (1, n=9)
[0055] Put 0.1mol 4-nonylphenol, 50ml n-hexane and 0.22mol (paraformaldehyde) into a 250ml reactor equipped with a constant pressure dropping funnel, a thermometer and a condenser tube (with a nitrogen bag), after 3 times of nitrogen replacement in the reactor , start to stir and heat up, and when the temperature rises to 40°C-45°C, start to drop 0.25mol of saturated aqueous solution of sodium hydroxide. After the dropwise addition, keep stirring and react for 5 hours. After the reaction is completed, wash with 2mol / L hydrochloric acid aqueous solution and water in turn Residual sodium hydroxide and paraformaldehyde were removed from the reaction solution, and the solvent was evaporated to dryness under reduced pressure to obtain compound I, which was directly put into the next reaction.
[0056] Compound I is 2,6-dimethylol-4-nonylphenol, a yellow solid, and its nuclear magnetic resonance spectrum...
Embodiment 2
[0057] Embodiment 2: the preparation of three poly-4-nonylphenols (II-1, n=9)
[0058] Put 0.1mol of 2,6-dimethylol-4-nonylphenol, 0.22mol of 4-nonylphenol and 60ml of xylene into a 250ml reactor equipped with a thermometer and a condenser tube (with nitrogen bag), under nitrogen protection Heat up to 60°C-70°C, stir quickly until the reaction system is evenly dispersed, then put in solid acid (2% of the mass fraction of 4-nonylphenol), heat up to reflux temperature and react for 4 hours, and cool down to 25°C-35°C after the reaction , filtered off the solid acid, evaporated to dryness under reduced pressure, and separated and purified by column chromatography to obtain compound II-1, trimerized-4-nonylphenol, a light yellow viscous substance, and its nuclear magnetic resonance spectrum data is:
[0059] 1 HNMR (400MHz, CDCl 3 )δ7.20(d,2H,ArH),7.07(d,2H,ArH),6.88(d,2H,ArH),6.73(d,2H,ArH),3.90(S,2H,CH 2 ),3.81(S,2H,CH 2 ),1.67-0.55(19H,C 9 h 19 ).
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