A kind of hydrophilic stone cultural relics nano protective agent and preparation method thereof
A technology of stone cultural relics and protective agent, applied in antifouling/underwater coatings, paints containing biocides, coatings, etc., which can solve the problems of blocking the gaps of cultural relics, hindering the normal movement of water and gas, and protective damage.
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Embodiment 1
[0066] The synthesis method of nano-silica is:
[0067] (1) Synthesis of star macromolecular initiator 21Br-β-CD:
[0068] Take 6.82g β-cyclodextrin, dry it at 80°C for 12h under vacuum conditions, then dissolve it in 60mL of N-methylpyrrolidone at room temperature, put it in an ice-water bath, and cool it to 0°C. 58g of 2-bromoisobutyryl bromide was added dropwise within 2h, the temperature was raised to room temperature after the dropwise addition was completed, and the reaction was continued for 24h to obtain a brown solution, which was concentrated by distillation under reduced pressure, diluted by adding 100mL of dichloromethane, and respectively with 100mL of saturated aqueous sodium bicarbonate solution. and 100 mL of deionized water were washed three times each, the obtained organic phase was dried with anhydrous magnesium sulfate, then concentrated with a rotary evaporator, and finally precipitated in n-hexane below -20 ° C to obtain a white precipitate, which was pla...
Embodiment 2
[0084] A method for synthesizing nano-silver, the steps of which are similar to those of nano-silicon dioxide, except that nano-silver is synthesized by combining the synthesized multi-arm star block copolymer β-CD-g-[PAA-b- PEG] and the precursor AgNO 3 The reaction steps are:
[0085] Dissolve 10 mg of multi-arm star block copolymer β-CD-g-[PAA-b-PEG] in 10 mL of DMF to prepare a monomolecular micelle template solution; then add 58.9 mg of AgNO 3 And 2mL of ethanol, react at 100 ℃ for 10h, that is.
[0086] TEM image of silver nanoparticles figure 1 As shown, it can be seen that the size of the nanoparticles is uniform, and the average particle size is about 10 nm.
[0087] The solubility of silver nanoparticles in water was tested, and the results were as follows figure 2 As shown, it can be seen that the silver nanoparticles prepared by the present invention have good solubility.
Embodiment 3
[0089] A hydrophilic nanometer protective agent for stone cultural relics, comprising the following raw materials in parts by weight: 5 parts of nano-silicon dioxide, 0.5 parts of nano-silver, 30 parts of propylene glycol, 5 parts of fluorine surfactant FC-4430, wetting agent 0.2 part of PE-100, 0.3 part of Nopco SN50400, 0.2 part of Nopoco NXZ, 0.1 part of preservative CP-19, and 58.7 parts of water.
[0090] The preparation method of the hydrophilic stone cultural relic nano-protector comprises the following steps:
[0091] (1) Dispersion: Add propylene glycol to the dispersion tank, add water-based wetting agent, water-based dispersant, water-based defoamer, and CP-19 preservative under stirring conditions, continue stirring at low speed for 10 minutes, and then add nano-diol under stirring conditions. Silicon oxide and nano-silver, and continue to stir for 30min to obtain nano-dispersion;
[0092] (2) Compounding: add water to the stainless steel reaction kettle, add the ...
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