Specific embodiment
Below by specific embodiment, the preparation method of the hydroxyl endblocked polydimethylsiloxane that viscosity is controlled is described, the present embodiment is not limited to following examples.
Embodiment 1
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin and gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50~120 ℃ of dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 100 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes low molecule and extremely flows out without cut under suitable temperature and vacuum tightness, namely get transparent well, viscosity is 74000~80000 107 silicon rubber.
Embodiment 2
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 100 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 70000~75000 107 silicon rubber.
Embodiment 3
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 20ppm reagent A (reagent A is Silver Nitrate), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 66000~73000 107 silicon rubber.
Embodiment 4
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of ℃ of temperature, add 30ppm reagent A (reagent A is calcium sulfite), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 55000~68000 107 silicon rubber.
Embodiment 5
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 47000~56000 107 silicon rubber.
Embodiment 6
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin and gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 0.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 42000~50000 107 silicon rubber.
Embodiment 7
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is anionite-exchange resin), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 39000~46000 107 silicon rubber.
Embodiment 8
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is Silver Nitrate), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 37000~42000 107 silicon rubber.
Embodiment 9
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is calcium sulfite), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 130 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 35000~39000 107 silicon rubber.
Embodiment 10
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 32000~36000 107 silicon rubber.
Embodiment 11
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 20ppm reagent A (reagent A is calcium sulfite and gac), add 20ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 55ppmKOH alkali glue after material dewatering, the polymerization that heats up under 120 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 20000~29000 107 silicon rubber.
Embodiment 12
Hydrolyzate pre-treatment: add 300g hydrolyzate and 200g water in the there-necked flask of 500mL, stir 30min at 50 ~ 75 ℃ of temperature, add 30ppm reagent A (reagent A is calcium sulfite and gac), add 30ppm reagent B after stirring 30min, regulate pH=7.1, stop stirring, standing, separate, obtain required hydrolyzate.
Alkali glue preparation: add 150gDMC in the 250mL there-necked flask, add 5.5gKOH after 50 ℃~120 ℃ dehydrations, carry out polymerization in 130 ~ 150 ℃ and obtain KOH alkali glue.
107 silicon rubber are synthetic: will add through the hydrolyzate of pre-treatment in the 500mL reactor, heat up, dewater under vacuum, add 30ppmKOH alkali glue after material dewatering, the polymerization that heats up under 140 ℃, reaction system add the phosphate aqueous solution neutralization when arriving required viscosity, after neutralization, system removes under suitable temperature and vacuum tightness and flows out without cut low dividing to treating, namely get transparent well, viscosity is 20000~25000 107 silicon rubber.