CN102030990A - Silicone oil microcapsule with slow-release characteristics and preparation method thereof - Google Patents
Silicone oil microcapsule with slow-release characteristics and preparation method thereof Download PDFInfo
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Abstract
The invention provides a silicone oil microcapsule with slow-release characteristics and a preparation method thereof, relating to the field of new chemical materials. In the invention, ethyl orthosilicate or methyl orthosilicate, non-functional linear silicone oil and silane coupling agents with long-chain alkyl are used as oil phases, silicone oil microcapsule dispersion liquid taking silicon dioxide as a shell is prepared by the following steps of: compounding anionic surface active agents with nonionic surface active agents into emulsifying agents; carrying out ultrasonic emulsification to obtain miniemulsion; stirring at room temperature for hydrolysis; and finally regulating pH value; wherein the silicone oil microcapsule dispersion liquid taking silicon dioxide has grain diameter of 140-260 nanometers and solid content of 13%-20%. The silicone oil microcapsule has high storage stability and good slow-release characteristics and can be directly used for the preparation of high-durability hydrophobic coating.
Description
Technical field
The present invention relates to the new chemical materials field, be specifically related to a kind of silicone oil microcapsule and preparation method thereof with slow release characteristic.
Background of invention
Prior art discloses silicone oil and has had that viscosity-temperature coefficient is little, high-low temperature resistant, anti-oxidant, lightning is high, volatility is little, good insulating, surface tension are little, metal is not had characteristics such as burn into is nontoxic, steam forces down, and can be used for senior lubricant, transformer oil, defoamer, releasing agent, optical brightener, antifouling paint etc.Studies show that the microcapsule that contain silicone oil also can be used for high-efficient corrosion inhibitor, organic pollutant extraction agent, biooxidation reactions holder, slowly-releasing hydrophobizing agent, slowly-releasing stain control agent of weapon etc. except such use.At present, the preparation method of silicone oil microcapsule has emulsion polymerization, situ aggregation method, solvent evaporated method etc., adopting emulsion polymerization to prepare polyacrylic resin as Japanese Patent JP2007034156-A is the silicone oil microcapsule of shell, can be used for the preparation of ink powder after the drying; Luo etc. (J.Microencapsul.2008,25,196-202) adopting solvent evaporated method to prepare is the silicone oil microcapsule of shell with the polysulfones, is used for the toxic volatile treatment of organic matters of organic of water; It is the silicone oil microcapsule of shell with the urea-formaldehyde resin that Huang Zhenya (Huang Zhenya, Institutes Of Technology Of Nanjing's Master's thesis, 2008) adopts situ aggregation method to prepare, and can reduce the ablation of propelling charge to the weapon barrel effectively.But above-mentioned silicone oil microcapsule are housing with organic resin (as polyacrylic resin, urea-formaldehyde resin, polyamide resin, polysulfone resin) all, exist complicated process of preparation, the feature of environmental protection not good, and shortcoming such as silicone oil microcapsule wall poor heat resistance.
Summary of the invention
The objective of the invention is for overcoming the defective of prior art, provide a kind of preparation technology simple, safety non-toxic, excellent performance, silicone oil microcapsule with sustained release performance, silicone oil microcapsule of the present invention can be directly as the slowly-releasing hydrophobic additive of water-borne coatings, gives the persistent waterproof of coating, function such as anti-icing, antifouling.
On the other hand, the invention provides a kind of novel method that in water-based system, prepares the silicone oil microcapsule.
Silicone oil microcapsule of the present invention are with silicone oil, tetraethoxy (TEOS) or methyl silicate (TMOS) and to contain the mixture that the silane coupling agent of chain alkyl forms be oil phase, with the anionic/nonionic surfactant compound is emulsifying agent, makes the silicone oil micro-capsule dispersion liquid of energy stably stored by pre-emulsification, ultrasonic thin emulsification, pH regulator, stirring at room hydrolysis.Wherein the shell of silicone oil microcapsule is a silicon-dioxide, is to form at oil/water termination generation hydrolytie polycondensation by TEOS in the miniemulsion drop (or TMOS) and silane coupling agent, has hole in the shell, for the silicone oil molecule provides passage to external diffusion.
The silicone oil microcapsule particle diameter 140-260nm that the present invention makes, shell thickness 10-40nm, the solid content of silicone oil dispersion liquid are 10%-30%, preferred solid content 13%-20%.
The used silicone oil of the present invention is the line style silicone oil of non-functional group, and as dimethyl silicone oil, diethyl silicone oil, methyl phenyl silicone oil etc., consumption is 3-10wt%.
Silane coupling agent of the present invention contains at least one chain alkyl and at least one alkoxyl group, the methyl in the chain alkyl and methylene radix 〉=16.The alkyl segment plays the ligation between silica shell and the silicone oil nuclear, and segment is too short, and silicon-dioxide can not effectively be coated on the surface of silicone oil drop.Alkoxy base can make silane coupling agent and TEOS (or TMOS) that copolycondensation takes place.This type of silane coupling agent comprises: hexadecyl Trimethoxy silane, octadecyl Trimethoxy silane, hexadecyl triethoxyl silane, octadecyltriethoxy silane etc., the ratio of TEOS and silane coupled agent content total amount and silicone oil is about 0.5: 1-1: 1 (weight ratio).
The present invention adopts the emulsion stabilizer of aniorfic surfactant and the initial miniemulsion drop of the composite conduct of nonionogenic tenside, the proportional range of anionic/nonionic emulsifier is 0.2: 1-1: 1 (weight ratio), wherein anionic emulsifier is one or more in the aniorfic surfactant such as sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate, and nonionic emulsifier is one or more in the nonionic surface active agent such as alkylphenol polyoxyethylene, high-carbon fatty alcohol polyoxyethylene ether.The proportional range of tensio-active agent total amount and oil phase is 0.1: 1-0.3: 1.
Ultrasonic thin emulsive time range of the present invention is 10-30 minute.Ultrasonic time is too short, and thin emulsification is insufficient, the easy unstability of emulsion; Ultrasonic time is long, and the oxide of high activity silicone content that the miniemulsion drip gauge is looked unfamiliar increases, and easily produces demulsifying phenomenon when ultrasonic.
The present invention need adopt pH value conditioning agent that the pH value of miniemulsion is adjusted to 7-8, and the adjusting of pH value is after ultrasonic thin emulsification finishes opportunity, regulates the pH value in other stage and all is difficult to obtain stable silicone oil micro-capsule dispersion liquid.The pH regulator agent of being adopted is alkali, carbonate, supercarbonate, hydrophosphate, phosphoric acid salt or the hydrosulfate etc. of basic metal, alkaline-earth metal or ammonium, as sodium bicarbonate, yellow soda ash, potassiumphosphate, sal enixum etc.
Miniemulsion hydrolysis process condition of the present invention is: stirring at room 24-48h.
The silicone oil microcapsule that the present invention obtained, can be directly as the hydrophobic additive of water-borne coatings, the coating that has functions such as persistent waterproof, anti-icing, anti-pollution flashover with preparation.
The preparation method of the silicone oil microcapsule with slow release characteristic that the present invention proposes has the following advantages:
Technology is simple, cost is low, reaction conditions is gentle, be easy to control.Be reflected in the aqueous medium and carry out, do not contain organic solvent, safety non-toxic fully.The silicone oil micro-capsule dispersion liquid concentration height that makes, good stability can directly be filled among the water-borne coatings.
The slow release characteristic of silicone oil microcapsule of the present invention is to measure by the hydrophobic persistence of the coating of its filling.Be specially: silicone oil microcapsule and color stuffing, auxiliary agent, emulsion are made into coating, be coated on the base material, drying, the initial water of testing coating (2 μ L) contact angle, at room temperature, utilize tap water to wash away (rain drop erosion in simulating nature circle) coating continuously 2 hours, then 80 ℃ dry 12 hours down, test water contact angle, and then wash away with tap water, circulate with this, wash away the hydrophobic persistence that the variation of coating water contact angle under the number of times reflects coating by measuring difference.
The silicone oil microcapsule median size that the present invention makes is measured by the laser particle diameter tester of the Coulter N4 Plus of U.S. Beckman company, and silicone oil microcapsule pattern is observed by the Hitachi H-600 transmission electron microscope (TEM) of Japanese Hitachi company and obtained.
For the ease of understanding, below will the present invention be described in detail by concrete drawings and Examples.It needs to be noted, specific embodiments and the drawings only are in order to illustrate, obviously those of ordinary skill in the art can illustrate according to this paper, within the scope of the invention the present invention is made various corrections and change, and these corrections and change are also included in the scope of the present utility model.
Description of drawings
Fig. 1 is silicone oil microcapsule transmission electron microscope (TEM) figure of embodiment 1 preparation, and the microcapsule particle diameter is about 200nm.
Fig. 2 is silicone oil microcapsule transmission electron microscope (TEM) figure of embodiment 3 preparations, and the microcapsule particle diameter is about 210nm.
Fig. 3 is the water contact angle of the coating of embodiment 3 and comparative example 1 gained washes away number of times with tap water a variation diagram.
Embodiment
Embodiment 1:
0.25 gram sodium laurylsulfonate and 0.75 gram high-carbon fatty alcohol polyoxyethylene ether are dissolved in the 100 gram deionized waters, add the oil mixture of forming by 10 gram dimethyl silicone oils, 10 gram TEOS, 1 gram octadecyl Trimethoxy silane again, pre-emulsification was stirred 15 minutes under ice water bath environment, use the cell pulverization machine to carry out ultrasonic thin emulsification 20 minutes then, obtain miniemulsion.The pH value of miniemulsion is adjusted to 7.5, and high-speed stirring is 24 hours under the normal temperature, gets oyster white silicone oil microcapsule suspensions.
With above-mentioned silicone oil microcapsule suspensions 3.91 grams, water 10 grams, organosilicon crylic acid latex (solid content 46%) 3.76 grams, titanium dioxide 3 grams, BYK-1540.06 gram are mixed with coating, apply, drying at room temperature 12h, hydrophobic coating.
Embodiment 2:
0.25 gram sodium laurylsulfonate and 0.75 gram alkylphenol polyoxyethylene are dissolved in the 100 gram deionized waters, add the oil mixture of forming by 10 gram dimethyl silicone oils, 7 gram TEOS, 1.5 gram hexadecyl Trimethoxy silanes again.Pre-emulsification was stirred 15 minutes under ice water bath environment, used the cell pulverization machine to carry out ultrasonic thin emulsification 20 minutes then, obtained miniemulsion.The pH value of miniemulsion is adjusted to 8, and high-speed stirring is 24 hours under the normal temperature, gets oyster white silicone oil microcapsule suspensions.
With above-mentioned silicone oil microcapsule suspensions 3.25 grams, water 10 grams, organosilicon crylic acid latex (solid content 46%) 3.11 grams, titanium dioxide 3 grams, BYK-1540.06 gram are mixed with coating, apply, drying at room temperature 12h, hydrophobic coating.
Embodiment 3:
0.25 gram sodium laurylsulfonate and 0.75 gram alkylphenol polyoxyethylene are dissolved in the 100 gram deionized waters, add the oil mixture of forming by 10 gram dimethyl silicone oils, 10 gram TEOS, 1.5 gram octadecyl Trimethoxy silanes again, pre-emulsification was stirred 15 minutes under ice water bath environment, use the cell pulverization machine to carry out ultrasonic thin emulsification 20 minutes then, obtain miniemulsion.The pH value of miniemulsion is adjusted to 7.5, and high-speed stirring is 24 hours under the normal temperature, gets oyster white silicone oil microcapsule suspensions.
With above-mentioned silicone oil microcapsule suspensions 3.41 grams, water 10 grams, organosilicon crylic acid latex (solid content 46%) 3.26 grams, titanium dioxide 3 grams, BYK-1540.06 gram are mixed with coating, apply, drying at room temperature 12h, hydrophobic coating.
Comparative example 1:
0.25 gram sodium laurylsulfonate and 0.75 gram alkylphenol polyoxyethylene are dissolved in the 100 gram deionized waters, add again in the 10 gram dimethyl silicone oils, pre-emulsification was stirred 15 minutes under ice water bath environment, used the cell pulverization machine to carry out ultrasonic thin emulsification 20 minutes then, obtained miniemulsion.The pH value of miniemulsion is adjusted to 7.5, and high-speed stirring is 24 hours under the normal temperature, gets translucent silicone oil emulsion.
With above-mentioned silicone oil microcapsule suspensions 2.82 grams, water 10 grams, organosilicon crylic acid latex (solid content 46%) 3.26 grams, titanium dioxide 3 grams, BYK-1540.06 gram are mixed with coating, apply, drying at room temperature 12h, hydrophobic coating.
Claims (12)
1. silicone oil microcapsule with slow release characteristic, it is characterized in that with silicone oil, tetraethoxy or methyl silicate and containing the mixture that the silane coupling agent of chain alkyl forms is oil phase, with the anionic/nonionic surfactant compound is emulsifying agent, the silicone oil micro-capsule dispersion liquid that makes by pre-emulsification, ultrasonic thin emulsification, pH regulator, stirring at room hydrolysis, the shell of described silicone oil microcapsule is a silicon-dioxide, silicone oil microcapsule particle diameter 140-260nm, shell thickness 10-40nm, the solid content of silicone oil dispersion liquid are 10%-30%.
2. the silicone oil microcapsule with slow release characteristic according to claim 1, its characteristic is, the shell of described silicone oil microcapsule forms at oil/water termination generation hydrolytie polycondensation by the tetraethoxy in the miniemulsion drop or methyl silicate and silane coupling agent, has hole in the shell.
3. the silicone oil microcapsule with slow release characteristic according to claim 1, its characteristic are that the solid content of described its silicone oil dispersion liquid of silicone oil microcapsule is 13%-20%.
4. the silicone oil microcapsule with slow release characteristic according to claim 1, its characteristic are that used silicone oil is the line style silicone oil of non-functional group.
5. the silicone oil microcapsule with slow release characteristic according to claim 4, its characteristic is that used silicone oil is selected from dimethyl silicone oil, diethyl silicone oil or methyl phenyl silicone oil.
6. the silicone oil microcapsule with slow release characteristic according to claim 1 is characterized in that described silane coupling agent contains at least one chain alkyl and at least one methoxy or ethoxy, the methyl in the chain alkyl and methylene radix 〉=16.
7. the silicone oil microcapsule with slow release characteristic according to claim 1 is characterized in that described anionic emulsifier is selected from one or more in the aniorfic surfactant such as sodium lauryl sulphate, sodium laurylsulfonate, Sodium dodecylbenzene sulfonate; Described nonionic emulsifier is selected from one or more in alkylphenol polyoxyethylene or the high-carbon fatty alcohol polyoxyethylene ether.
8. the silicone oil microcapsule with slow release characteristic according to claim 1, the ratio that it is characterized in that anionic/nonionic emulsifier is 0.2: 1-1: 1 weight ratio.
9. the silicone oil microcapsule with slow release characteristic according to claim 1 is characterized in that the described ultrasonic thin emulsive time is 10-30 minute.
10. the silicone oil microcapsule with slow release characteristic according to claim 1, the pH value when it is characterized in that described miniemulsion hydrolysis is adjusted to 7-8.
11. the silicone oil microcapsule with slow release characteristic according to claim 1 is characterized in that described miniemulsion hydrolysis process condition is: stirring at room 24-48h.
12. the purposes of the silicone oil microcapsule of claim 1 in the preparation hydrophobic coating.
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