A kind of preparation method of anionic linear copolymerization organosilicon softening agent
A softening finishing agent, anionic technology, applied in the field of preparation of anionic linear copolymer silicone softening finishing agent, can solve the problems of low foam rate, unusable dyeing system, stable work, etc., to improve alkali resistance and compatibility. sex, overcoming the "greasy effect"
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[0051] The preparation method of anionic linear copolymerization organosilicon softening agent, its steps are as follows:
[0052] ⑴ Preparation of double-ended hydrogen-containing silicone oil
[0053] 1,1,3,3-Tetramethyldisiloxane and octamethylcyclotetrasiloxane and / or dimethylcyclotetrasiloxane at 1.0-10.0%: 90.0-99.0% (mass percentage) put into the stirred tank, add 1.0-3.0% of the acidic catalyst by the weight of the above two raw materials, stir and react for 3-9 hours at a temperature of 25-75°C, carry out the ring-opening chain extension reaction, remove the acidic catalyst, and then raise the temperature to 90 ~140°C vacuumizes to separate the low-boiling point substances to obtain double-ended hydrogen-containing silicone oil with a viscosity (25°C) of 100-1000 mpa.s, and its content is at least 95.0%.
[0054] ⑵ Preparation of double-ended chlorine-containing silicone oil
[0055] The molar ratio of double-ended hydrogen-containing silicone oil and methallyl chlo...
Embodiment 1
[0067] ⑴ Preparation of double-ended hydrogen-containing silicone oil
[0068] Put 8 grams of 1,1,3,3-tetramethyldisiloxane and 190 grams of octamethylcyclotetrasiloxane into a 500ml four-neck round bottom flask, add 5 grams of concentrated sulfuric acid, Stir the reaction for 7-9 hours, carry out the ring-opening chain extension reaction, use the sedimentation method to remove the concentrated sulfuric acid, then raise the temperature to 90-140°C and vacuumize for 3-5 hours, separate the low boiling point substances, and obtain a viscosity (25°C) of 100-140mpa.s The content of double-ended hydrogen-containing silicone oil is 95.0-96.5%.
[0069] ⑵ Preparation of double-ended chlorine-containing silicone oil
[0070] 100 gram double-end hydrogen-containing silicone oils and 4.5 gram methallyl chlorides that step 1 makes are dropped in 250ml four-neck round-bottomed flasks, drop into 3 gram chloroplatinic acid alcohol solutions (10% mass percent isopropyl chloroplatinic acid ...
Embodiment 2
[0084] 100 grams of octamethylcyclotetrasiloxane (D 4 ) into 100 grams of dimethylcyclosiloxane (DMC), 5 grams of vitriol oil in step (1) and (3) are changed into 4 grams of trifluoromethanesulfonic acid, and undecylenic acid in step (4) is changed into dodecene acid, polyethylene glycol 600 in step (6) is replaced with polyether 600 (EO / PO mixed polymerization, wherein p=11, q=1), and the platinum catalyst in step (2) and (4) adopts polyether 600 in dimethylsiloxane For 1,3-divinyl-1,1,3,3-tetramethyldisiloxane platinum complex, the solvent in step (7) isopropanol was changed to ethylene glycol butyl ether, and the rest were the same as in Example 1.
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