Long service life and large color difference organic reversible thermochromic microcapsules and preparation method
A thermochromic, long-life technology, used in microcapsule preparations, microsphere preparation, color-changing fluorescent materials, etc., can solve the problems of small color difference, poor light transmittance, short service life, etc. big effect
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[0048] The preparation method of long-color large organic reversible thermochromic microcapsules includes the following steps:
[0049] a) Add an oil-soluble initiator to the monomer A or the mixture of monomer A and monomer C for prepolymerization,
[0050] b) Add organic reversible thermochromic compound after prepolymerization,
[0051] c) Add monomer B and disperse it into an oil-in-water emulsion in an aqueous solution containing a dispersant,
[0052] d) Carry out free radical polymerization reaction, filter, wash and dry to obtain organic reversible thermochromic microcapsules.
[0053] The initiator is preferably azobisisobutyronitrile, the amount of the initiator is preferably 0.5-2% by weight of the monomer A, the prepolymerization temperature is between 60°C and 70°C, and the prepolymerization time is 30 minutes.
[0054] Acrylate and / or methacrylate contains carbon-carbon double bonds in the molecule, and the groups connected to the unsaturated bonds have greater polarity, so...
Embodiment 1
[0059] Example 1. Weigh 10.0 g of refined methyl methacrylate (MMA) with an electronic balance into a three-necked flask, add 0.10 g of initiator azobisisobutyronitrile (AIBN), and prepolymerize at 65°C in a water bath 30min, add 10.0 g of organic reversible thermochromic compound, add 1.00 g of divinylbenzene (DVB), the ratio of organic reversible thermochromic compound is 3,3-bis(4-dimethylaminophenyl)- The ratio of 6-dimethylaminophthalide: 4,4'-dihydroxydiphenyl sulfone: 1-hexadecanol is 1:3:150, and 200 grams of the mixture is added to a concentration of 0.3% polyvinyl alcohol ( In the PVA) aqueous solution, use a high-shear emulsifier to shear and emulsify for 3 minutes, then increase the temperature to 75°C, continue the reaction for 3 hours, and then increase the temperature to 85°C for 1 hour. The product is washed, filtered, and dried to obtain microcapsule product powder.
Embodiment 2
[0060] Example 2. Using an electronic balance, weigh 10.0 grams of refined methyl methacrylate (MMA) and 0.20 grams of methacrylic acid (MAA) into a three-necked flask, and add 0.10 grams of initiator azobisisobutyronitrile (AIBN) , Prepolymerize for 30min under 65℃ water bath condition, add 10.0g of thermochromic compound, add 1.50g of divinylbenzene, the ratio of organic reversible thermochromic compound is 3,3-bis(4-dimethylamino) (Phenyl)-6-dimethylaminophthalide: 4,4'-dihydroxydiphenyl sulfone: 1-hexadecanol with a ratio of 1:3:150, and add 200 grams of the mixture to a concentration of 0.3% by weight In the aqueous solution of polyvinyl alcohol (PVA), use a high-shear emulsifier to shear and emulsify for 3 minutes, then increase the temperature to 75°C, continue the reaction for 3 hours, and then increase the temperature to 85°C for 1 hour. The product is washed, filtered, and dried to obtain microcapsule product powder.
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