A kind of cross-linked silicone slip agent and preparation method thereof
A technology of slip agent and silicone, applied in the direction of coating, etc., can solve the problems of excessive recoating performance and reduction of paint foam, and achieve the effects of reduced surface tension, good leveling and excellent hand feeling
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Embodiment 1
[0027] Step 1: Add 90g of polydimethylsiloxane with a viscosity of about 20mcSt, 68g of hydrogen-containing tetramethylcyclotetrasiloxane (hydrogen-containing D4), 300ml of isobutanol, and 0.5g of acetic acid as catalysts into a condenser In a three-necked flask with a thermometer, under nitrogen, they were heated to 85°C for 2 hours, and then at 85°C and under reduced pressure (-101.325kPa), the reaction mixture was degassed for 4 hours. The low molecular weight substances were removed from the product, thereby preparing the intermediate product I(A1). The viscosity of A1 at 40°C is 601356 mPa·s, the molecular weight is about 263000, and the degree of polymerization is 3552.
[0028] According to the infrared spectrogram:
[0029] 1056.8cm -1 Indicates that it contains Si-O; 1010.3cm -1 Indicates that it contains Si—C; 1257.5cm -1 、785.8cm -1 Indicates that it contains Si—CH 3 , Si—(CH 3 ) 3 Structure; 2963cm -1 Indicates that it contains a methyl structure; at 3400-...
Embodiment 2
[0039] Step 1: Use 109g of polydimethylsiloxane with a viscosity of about 50mcSt, 68g of hydrogen-containing tetramethylcyclotetrasiloxane (hydrogen-containing D4), 350ml of isobutanol, and 1.3g of 98% methanesulfonic acid as catalysts Add in a three-necked flask equipped with a condenser and a thermometer, and under nitrogen, heat them to 85°C over 2 hours, then degas the reaction mixture for 4 hours at 85°C and reduced pressure (-101.325kPa), and react After completion, low-molecular-weight substances were removed from the reaction product, thereby producing an intermediate product I(A2). The viscosity of A2 at 25° C. is 993,700 mPa·s, the molecular weight is about 303,414, and the degree of polymerization is 4,098.
[0040] According to the infrared spectrogram:
[0041] 1053.2cm -1 Indicates that it contains Si-O; 1021.3cm -1 Indicates that it contains Si—C; 1307.6cm -1 、806.1cm -1 Indicates that it contains Si—CH 3 , Si—(CH 3 ) 3 Structure; 2889cm -1 Indicates th...
Embodiment 3
[0051] Step 2: With N 2 Add 156g tetramethylcyclotetrasiloxane, 0.9g tetramethylammonium hydroxide and 273g modified ultra-high molecular weight polysiloxane (A2) in the reaction flask of conduit, thermometer and distillation head, pass N 2 Slowly heat up to 70°C and maintain for 1.8 hours. After the catalyst is completely dissolved, continue to heat up and react at 80°C for 7 hours. After the reaction is complete, raise the temperature to about 165°C and maintain for 2 hours. Add 23g of 0.01N hydrochloric acid aqueous solution and 123g of n-triacene under constant stirring, and hydrolyze the mixture for 2 hours at 65-75°C; 187g of modified ultrahigh molecular weight polysiloxane (B3) was obtained.
[0052]
[0053] According to the infrared spectrogram:
[0054] 1066.8cm -1 Indicates that it contains Si-O; 1023.2cm -1 Indicates that it contains Si—C; 1411.3cm -1 、766.1cm -1 Indicates that it contains Si—CH 3 , Si—(CH 3 ) 3 Structure; 2907cm -1 Indicates that it c...
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