Aminated intermediate, and aminated polyether and phosphorylated star-like products, preparation method and application thereof
An intermediate and amination technology, applied in the field of amination intermediates, can solve the problems of uncontrollable molecular structure and weight-average molecular weight of superplasticizers, uncontrollable side reactions of copolymerization, and easy chain transfer of phosphorus-containing groups.
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Embodiment 1
[0063] Preparation of Chlorinated Polyether M-1.
[0064] Weigh 1000 parts of methoxypolyether (M n =1000, d=18, e=3) into the reactor, under the condition of -0.08MPa~-0.1MPa, vacuumize for 1h to remove water and a little volatile components in the polyether. Cool down to 40~60℃, in N 2 Under protection conditions, add SOCl to the above reaction system 2 155 parts, the temperature of the reaction system is controlled not to exceed 60°C during the dropwise addition. After the dropwise addition is completed, connect the cooling reflux device, raise the temperature of the reaction system to 80-90°C, continue the heat preservation reaction for 3-5 hours, and then distill out the acidic volatile components in the reaction system under reduced pressure to obtain a light brown product, which is passed through Liquid phase test showed that the yield of chlorinated polyether M-1 was 99.1%. Similarly, the following chlorinated polyethers are prepared for the synthesis of aminated ...
Embodiment 2
[0072] Preparation of aminated intermediate N-1
[0073] Weigh 94 parts of phenol as a primer, gradually add 5853 parts of polyethyleneimine (a=45), stir evenly and then heat up to 60-80°C, weigh 162 parts of 37wt% formaldehyde, drop them completely within 2-4 hours, and then The temperature was raised to 85°C, and the reaction was kept for 6 hours. The obtained light brown liquid was tested by GPC, and the weight average molecular weight was 94+5853+14*3-6=5983, and the weight average molecular weight distribution was 1.78.
[0074] Similarly, the following aminated intermediates are prepared for the synthesis of aminated polyether intermediates.
[0075] N-2: 110 parts of hydroquinone, 3508 parts of polyethyleneimine (a=20), 389 parts of 37wt% formaldehyde, reaction temperature 95°C, reaction time 4h, light brown liquid, tested by GPC, weight average molecular weight It is 110+3508+14*4-8=3666, and the weight average molecular weight distribution is 1.75.
[0076] N-3: 10...
Embodiment 3
[0082] In a closed autoclave, use N-1 as the base, add 10833 parts of reaction solvent water, stir evenly, heat up to 60-80 °C, gradually add 30000 parts of chlorinated polyether M-1, then heat up to 100 °C, keep warm Reaction 8h.
[0083] After the reaction, cool down to 50°C-70°C, gradually add 5853 parts of catalyst concentrated hydrochloric acid, then add 9102 parts of phosphorous acid, and finally add 9000 parts of 37wt% formaldehyde, raise the temperature of the reaction to 100°C, and continue the heat preservation reaction for 30 hours to obtain reddish-brown Liquid, tested by GPC, the weight average molecular weight is 45352, PDI=3.41.
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