CN105733392A - Sub-micrometer polydivinylbenzene particles and high-temperature-resistant super-hydrophobic coating preparation method - Google Patents
Sub-micrometer polydivinylbenzene particles and high-temperature-resistant super-hydrophobic coating preparation method Download PDFInfo
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Abstract
The invention provides sub-micrometer polydivinylbenzene particles and a high-temperature-resistant super-hydrophobic coating preparation method.The preparation method includes the steps of 1, conducting miniemulsion polymerization to obtain nanometer emulsion I; 2, conducting seeded emulsion polymerization to obtain sub-micrometer emulsion II; 3, displacing media of the emulsion II into low-boiling-point solvents by water through centrifugation or freeze drying, pouring or brushing a newly prepared coating on a substrate according to specific solid content, and obtaining a non-cracking super-hydrophobic coating with a certain film thickness after the coating is dried.The prepared super-hydrophobic coating is highly resistant to high temperature and has quite high contact angle after being subjected to high temperature treatment, and the non-cracking super-hydrophobic coating can be prepared by controlling the film thickness.The preparation method has the advantages of mild coating preparation conditions, environment friendliness, low raw material cost, simple operation technologies and no need for special machines and devices.
Description
Technical field
The present invention relates to a kind of super hydrophobic coating, be specifically related to a kind of submicron order polydivinylbenezene particle and there is high temperature resistant and super-hydrophobicity coating production.
Background technology
When the contact angle of water droplet and the surface of solids is more than 150 °, this surface of solids is referred to as super hydrophobic surface.Owing to super hydrophobic surface has special micro-rough structure with low surface energy, dirt is not easy at surface aggregation, also easily depart under the effect of gravity, wind-force or rainwater even if assembling, this gives the performance that super hydrophobic material is much excellent, such as waterproof, antifog, frost protection, anticorrosion, automatically cleaning etc., so that it is in automatically cleaning building coating, submerged structure anticorrosion, the aspects such as fabric is antifouling have broad application prospects.
Owing to super hydrophobic surface all has very important application prospect in theoretical research and actual industrial and agricultural production and daily life, therefore, the structure of the super-hydrophobic surface of solids causes to be paid close attention to widely.The construction method of super hydrophobic surface mainly has two: the first modifies low-surface energy substance in coarse substrate, mostly is fluorinated silicone modified resin；It two is build at hydrophobic surface to have the surface fine structure of certain roughness.Concrete grammar mainly has electrochemical etching, vapour deposition, electrostatic spinning etc., and above method needs special equipment mostly, and process is complex, and energy consumption and cost are of a relatively high.
Existing method prepares the super hydrophobic surface poor resistance to high temperature.Fluorine-containing material itself is expensive and fluorine material can be detrimental to health, to environment, and the super-hydrophobic coat formed by micro-and nano-particles easily ftractures, and causes contact angle to reduce.
Summary of the invention
The invention provides a kind of technique simple, high temperature resistant, do not ftracture, floride-free without silicon, with low cost, the preparation method of green super-hydrophobic coat.
The invention provides a kind of submicron order polydivinylbenezene particle and have high temperature resistant and super-hydrophobicity coating production, step is as follows:
Step 1: mini-emulsion polymerization
Under-5-20 DEG C of condition, divinylbenzene is added drop-wise in the solution of emulsifying agent, co-stabilizer and deionized water composition, is warming up to 30 80 DEG C after ultrasonic disperse, initiator is joined in above-mentioned mixed solution, stir 1 24 hours, prepare nanoscale emulsion I；Divinylbenzene in described mini-emulsion polymerization: emulsifying agent: co-stabilizer: initiator: the mass ratio of deionized water is 1:0.01 0.1:0.06 1.0:0.001 0.1:1 20；
Step 2: seeded emulsion polymerization
Divinylbenzene and emulsifying agent carry out pre-emulsification obtain pre-emulsion, pre-emulsion and initiator solution and be simultaneously added dropwise in nanoscale emulsion I 1-24 hour prepared submicron order emulsion II of reaction respectively；The divinylbenzene of pre-emulsion in described seeded emulsion polymerization: emulsifying agent: the mass ratio of deionized water is 1:0.01-0.1:1-20；Initiator in initiator solution in described seeded emulsion polymerization: the mass ratio of deionized water is 0.005-0.1:1-20；The volume of pre-emulsion: the volume of initiator solution: the volume ratio 1:0.01-1:1-20 of nanoscale emulsion I；
Step 3: the water in submicron order emulsion II is replaced as low boiling point solvent by centrifugal or lyophilization, obtain freshly prepd coating III, again freshly prepd coating III cast with the solid content of 0.5-10wt% or brush on base material, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture that thickness is 5 10 μm, be submicron order polydivinylbenezene particle and there is high temperature resistant and super-hydrophobicity coating.
Described emulsifying agent is one or more mixing in dodecyl sodium sulfate, dodecylbenzene sodium sulfonate, sodium lauryl sulphate or sodium stearate；
Described co-stabilizer is carbon number be 4 20 alkylol, carbon number be 4 20 fat alkane or one or more compound uses of polyvinyl alcohol；
Described initiator is the one in Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate-sodium bisulfite or hydrogen peroxide ferrous chloride.
In described step 3, low boiling point solvent includes aliphatic hydrocarbon and aromatic hydrocarbon, chlorohydrocarbon, alkylol and alkyl ketone etc..
Described base material is the conventional substrate materials such as piezoid, alloy, glass, pottery, leather, marble.
The preparation method of super-hydrophobic coat provided by the invention has the advantage that employing miniemulsion, seed emulsion, and special poly-method prepares polydivinylbenezene submicron particles, equipment is simple, and energy consumption is low, and cost is low, the low-surface energy substance such as fluorine silicon, environmental protection need not be added.
Super-hydrophobic coat provided by the invention has the advantage that the ultra-hydrophobicity of prepared super-hydrophobic coat is excellent, can keep stable performance under the high temperature conditions and can control coating and do not ftracture by controlling coating layer thickness.
Accompanying drawing explanation
The super-hydrophobic coat that the accompanying drawing embodiment of the present invention 1 provides.
Detailed description of the invention
The present invention is described in further details by combination technology scheme and accompanying drawing.
Embodiment 1
By 0.2g dodecyl sodium sulfate, 0.9g hexadecanol joins in 80ml deionized water, is cooled to less than 10 DEG C, drips 10g divinylbenzene after 50 DEG C of stirring 30min, after dropwising, it is cooled to 0 DEG C, ultrasonic disperse 3min, move in 50 DEG C of oil bath pans, 0.05g potassium peroxydisulfate is dissolved in 5ml deionized water, it is added drop-wise in system, 50 DEG C of reaction 10h, obtain nanoscale emulsion I.By 10g divinylbenzene, 0.35g dodecyl sodium sulfate is dissolved in and 30min is stirred at room temperature in 15ml water and obtains pre-emulsion, initiator 0.05g potassium peroxydisulfate is dissolved in 10ml water, emulsion I is warming up to 60 DEG C, pre-emulsion, initiator solution are simultaneously added dropwise in reaction bulb, dropping 5h, is warming up to 75 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.The medium of emulsion II is replaced as acetone by water by centrifugal, more freshly prepd coating is cast on piezoid with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 151 °.Placing 24h through 60 DEG C, contact angle is still greater than 150 °.
Embodiment 2
By 0.15g sodium lauryl sulphate, 0.8g hexadecanol joins in 75ml deionized water, is cooled to less than 10 DEG C, drips 10g divinylbenzene after 70 DEG C of stirring 30min, after dropwising, it is cooled to 0 DEG C, ultrasonic disperse 3min, move in 70 DEG C of oil bath pans, 0.05g ammonium persulfate-sodium bisulfite is dissolved in 5ml deionized water, it is added drop-wise in system, 70 DEG C of reaction 8h, obtain nanoscale emulsion I.By 8g divinylbenzene, 0.3g sodium lauryl sulphate is dissolved in and 30min is stirred at room temperature in 15ml water and obtains pre-emulsion, initiator 0.06g ammonium persulfate-sodium bisulfite is dissolved in 10ml water, emulsion I is warming up to 80 DEG C, pre-emulsion, initiator solution are simultaneously added dropwise in reaction bulb, dropping 3h, is warming up to 85 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.The medium of emulsion II is replaced as oxolane by water by lyophilization, more freshly prepd coating is cast on alloy with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 152 °.Placing 24h through 70 DEG C, contact angle is still greater than 150 °.
Embodiment 3
By 0.2g dodecylbenzene sodium sulfonate, 0.9g hexadecanol joins in 80ml deionized water, is cooled to less than 10 DEG C, drips 12g divinylbenzene after 80 DEG C of stirring 30min, dropwise, it is cooled to 0 DEG C, ultrasonic 3min, move in 80 DEG C of oil bath pans, 0.06g hydrogen peroxide ferrous chloride is dissolved in 5ml deionized water, it is added drop-wise in system, 80 DEG C of reaction 8h, obtain nanoscale emulsion I.By 9g divinylbenzene, 0.35g dodecylbenzene sodium sulfonate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.05g hydrogen peroxide ferrous chloride is dissolved in 15ml water, emulsion I is warming up to 80 DEG C, pre-emulsion, initiator solution are simultaneously added dropwise in reaction bulb, dropping 3h, is warming up to 85 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.The medium of emulsion II is replaced as acetone by water by lyophilization, more freshly prepd coating is brushed on glass with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 151 °.Placing 24h through 80 DEG C, contact angle is still greater than 150 °.
Embodiment 4
By 0.1g sodium lauryl sulphate, 0.3g hexadecanol, 0.4g hexadecane joins in 60ml deionized water, it is cooled to less than 10 DEG C after 60 DEG C of stirring 30min, dropping 7g divinylbenzene, dropwises, is cooled to 0 DEG C, ultrasonic 3min, move in 60 DEG C of oil bath pans, 0.05 potassium peroxydisulfate is dissolved in 5ml deionized water, is added drop-wise in system, 60 DEG C of reaction 10h, obtain nanoscale emulsion I.By 7g divinylbenzene, 0.35g sodium lauryl sulphate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.05g potassium peroxydisulfate is dissolved in 10ml water, emulsion I is warming up to 70 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb, dropping 5h, is warming up to 75 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.The medium of emulsion II is replaced as ethanol by water by lyophilization, more freshly prepd coating is cast on piezoid with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 150 °.Placing 24h through 100 DEG C, contact angle is still greater than 140 °.
Embodiment 5
By 0.2g sodium stearate, 0.4g hexadecanol, 0.5g hexadecane joins in 70ml deionized water, it is cooled to less than 10 DEG C after 70 DEG C of stirring 30min, dropping 13g divinylbenzene, dropwises, is cooled to 0 DEG C, ultrasonic 3min, move in 70 DEG C of oil bath pans, 0.05g ammonium persulfate-sodium bisulfite is dissolved in 5ml deionized water, is added drop-wise in system, 70 DEG C of reaction 8h, obtain nanoscale emulsion I.By 7g divinylbenzene, 0.35g sodium lauryl sulphate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.06g ammonium persulfate-sodium bisulfite is dissolved in 15ml water, emulsion I is warming up to 70 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb simultaneously, dropping 4h, is warming up to 75 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.By the medium of emulsion II by water by the centrifugal methanol that is replaced as, more freshly prepd coating is brushed on leather with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 152 °.Placing 24h through 60 DEG C, contact angle is still greater than 150 °.
Embodiment 6
By 0.1g dodecylbenzene sodium sulfonate, 0.7g hexadecane joins in 60ml deionized water, is cooled to less than 10 DEG C, drips 7g divinylbenzene after 60 DEG C of stirring 30min, dropwise, it is cooled to 0 DEG C, ultrasonic 3min, move in 60 DEG C of oil bath pans, 0.05g Ammonium persulfate. is dissolved in 5ml deionized water, it is added drop-wise in system, 60 DEG C of reaction 10h, obtain nanoscale emulsion I.By 6g divinylbenzene, 0.4g dodecylbenzene sodium sulfonate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.04g Ammonium persulfate. is dissolved in 15ml water, emulsion I is warming up to 75 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb, dropping 4h, is warming up to 85 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.By the medium of emulsion II by water by the centrifugal toluene that is replaced as, more freshly prepd coating is brushed on pottery with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 151 °.Placing 24h through 140 DEG C, contact angle is still greater than 130 °.
Embodiment 7
By 0.2g sodium stearate, 0.8g hexadecane joins in 85ml deionized water, is cooled to less than 10 DEG C, drips 12g divinylbenzene after 70 DEG C of stirring 30min, dropwise, it is cooled to 0 DEG C, ultrasonic 3min, move in 70 DEG C of oil bath pans, 0.05g hydrogen peroxide ferrous chloride is dissolved in 8ml deionized water, it is added drop-wise in system, 70 DEG C of reaction 9h, obtain nanoscale emulsion I.By 10g divinylbenzene, 0.35g sodium stearate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.05g hydrogen peroxide ferrous chloride is dissolved in 15ml water, emulsion I is warming up to 80 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb, dropping 3h, is warming up to 90 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.By the medium of emulsion II by water by the centrifugal oxolane that is replaced as, more freshly prepd coating is brushed on glass with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 151 °.Placing 24h through 120 DEG C, contact angle is still greater than 130 °.
Embodiment 8
By 0.2g dodecylbenzene sodium sulfonate, 0.9g polyvinyl alcohol joins in 70ml deionized water, is cooled to less than 10 DEG C, drips 13g divinylbenzene after 50 DEG C of stirring 30min, dropwise, it is cooled to 0 DEG C, ultrasonic 3min, move in 50 DEG C of oil bath pans, by molten for 0.07g potassium peroxydisulfate potassium sulfate solution in 10ml deionized water, it is added drop-wise in system, 50 DEG C of reaction 10h, obtain nanoscale emulsion I.By 7g divinylbenzene, 0.35g dodecylbenzene sodium sulfonate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.05g potassium peroxydisulfate is dissolved in 15ml water, emulsion I is warming up to 70 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb, dropping 4h, is warming up to 75 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.The medium of emulsion II is replaced as ethanol by water by centrifugal, more freshly prepd coating is cast on marble with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 151 °.Placing 24h through 110 DEG C, contact angle is still greater than 130 °.
Embodiment 9
By 0.15g dodecyl sodium sulfate, 0.8g polyvinyl alcohol joins in 60ml deionized water, is cooled to less than 10 DEG C, drips 10g divinylbenzene after 60 DEG C of stirring 30min, dropwise, it is cooled to 0 DEG C, ultrasonic 3min, move in 60 DEG C of oil bath pans, 0.05g Ammonium persulfate. is dissolved in 8ml deionized water, it is added drop-wise in system, 60 DEG C of reaction 9h, obtain nanoscale emulsion I.By 8g divinylbenzene, 0.3g dodecyl sodium sulfate is dissolved in and 30min is stirred at room temperature in 20ml water and obtains pre-emulsion, initiator 0.05g Ammonium persulfate. is dissolved in 10ml water, emulsion I is warming up to 80 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb, dropping 4h, is warming up to 85 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.The medium of emulsion II is replaced as acetone by water by lyophilization, more freshly prepd coating is cast on piezoid with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 151 °.Placing 24h through 80 DEG C, contact angle is still greater than 150 °.
Embodiment 10
By 0.1g sodium lauryl sulphate, 0.6g polyvinyl alcohol joins in 60ml deionized water, is cooled to less than 10 DEG C, drips 6g divinylbenzene after 70 DEG C of stirring 30min, dropwise, it is cooled to 0 DEG C, ultrasonic 3min, move in 70 DEG C of oil bath pans, 0.05g hydrogen peroxide ferrous chloride is dissolved in 5ml deionized water, it is added drop-wise in system, 70 DEG C of reaction 8h, obtain nanoscale emulsion I.By 7g divinylbenzene, 0.35g sodium lauryl sulphate is dissolved in and 30min is stirred at room temperature in 15ml water and obtains pre-emulsion, initiator 0.05g hydrogen peroxide ferrous chloride is dissolved in 15ml water, emulsion I is warming up to 85 DEG C, pre-emulsion and initiator solution are simultaneously added dropwise in reaction bulb, dropping 3h, is warming up to 90 DEG C of reaction 30min, obtains submicron order emulsion II after completion of dropwise addition.By the medium of emulsion II by water by the centrifugal chlorohydrocarbon that is replaced as, more freshly prepd coating is brushed on glass with certain solid content, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture of certain thickness.Contact angle is 152 °.Placing 24h through 130 DEG C, contact angle is still greater than 130 °.
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention being not restricted by the embodiments, other are any without departing from the change made under principles of the invention and spirit, are included in protection scope of the present invention.
Claims (10)
1. a submicron order polydivinylbenezene particle and there is high temperature resistant and super-hydrophobicity coating production, it is characterised in that step is as follows:
Step 1: mini-emulsion polymerization
Under-5-20 DEG C of condition, divinylbenzene is added drop-wise in the solution of emulsifying agent, co-stabilizer and deionized water composition, is warming up to 30 80 DEG C after ultrasonic disperse, initiator is joined in above-mentioned mixed solution, stir 1 24 hours, prepare nanoscale emulsion I；Divinylbenzene in described mini-emulsion polymerization: emulsifying agent: co-stabilizer: initiator: the mass ratio of deionized water is 1:0.01 0.1:0.06 1.0:0.001 0.1:1 20；
Step 2: seeded emulsion polymerization
Divinylbenzene and emulsifying agent carry out pre-emulsification obtain pre-emulsion, pre-emulsion and initiator solution and be simultaneously added dropwise in nanoscale emulsion I 1-24 hour prepared submicron order emulsion II of reaction respectively；The divinylbenzene of pre-emulsion in described seeded emulsion polymerization: emulsifying agent: the mass ratio of deionized water is 1:0.01-0.1:1-20；Initiator in initiator solution in described seeded emulsion polymerization: the mass ratio of deionized water is 0.005-0.1:1-20；The volume of pre-emulsion: the volume of initiator solution: the volume ratio 1:0.01-1:1-20 of nanoscale emulsion I；
Step 3: the water in submicron order emulsion II is replaced as low boiling point solvent by centrifugal or lyophilization, obtain freshly prepd coating III, again freshly prepd coating III cast with the solid content of 0.5-10wt% or brush on base material, to be coated after drying, obtain the super-hydrophobic coat that do not ftracture that thickness is 5 10 μm, be submicron order polydivinylbenezene particle and there is high temperature resistant and super-hydrophobicity coating.
2. coating production according to claim 1, it is characterised in that described emulsifying agent is one or more mixing in dodecyl sodium sulfate, dodecylbenzene sodium sulfonate, sodium lauryl sulphate or sodium stearate.
3. coating production according to claim 1 and 2, it is characterised in that described co-stabilizer is carbon number be 4 20 alkylol, carbon number be 4 20 fat alkane or one or more compound uses of polyvinyl alcohol.
4. coating production according to claim 1 and 2, it is characterised in that described initiator is the one in Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate-sodium bisulfite or hydrogen peroxide ferrous chloride.
5. coating production according to claim 3, it is characterised in that described initiator is the one in Ammonium persulfate., potassium peroxydisulfate, sodium peroxydisulfate, ammonium persulfate-sodium bisulfite or hydrogen peroxide ferrous chloride.
6. the coating production according to claim 1 or 2 or 5, it is characterised in that in described step 3, low boiling point solvent is oxolane, aliphatic hydrocarbon and aromatic hydrocarbon, chlorohydrocarbon, alkylol or alkyl ketone.
7. coating production according to claim 3, it is characterised in that in described step 3, low boiling point solvent is oxolane, aliphatic hydrocarbon and aromatic hydrocarbon, chlorohydrocarbon, alkylol or alkyl ketone.
8. coating production according to claim 4, it is characterised in that in described step 3, low boiling point solvent is oxolane, aliphatic hydrocarbon and aromatic hydrocarbon, chlorohydrocarbon, alkylol or alkyl ketone.
9. the coating production according to claim 1,2,5,7 or 8, it is characterised in that described base material is piezoid, alloy, glass, pottery, leather or marble.
10. coating production according to claim 6, it is characterised in that described base material is piezoid, alloy, glass, pottery, leather or marble.
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Cited By (4)
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| CN108359344A (en) * | 2018-01-19 | 2018-08-03 | 大连理工大学 | A kind of preparation method of high hydrophobicity high temperature resistant fluoresent coating |
| CN108409911A (en) * | 2018-01-19 | 2018-08-17 | 大连理工大学 | A kind of preparation method of super-hydrophobicity automatically cleaning fluoresent coating |
| CN109608689A (en) * | 2018-11-15 | 2019-04-12 | 华南理工大学 | A kind of super-hydrophobicity sponge and the preparation method and application thereof |
| CN116081623A (en) * | 2023-04-11 | 2023-05-09 | 华侨大学 | Super-hydrophobic activated carbon material and preparation method and application thereof |
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| CN108359344A (en) * | 2018-01-19 | 2018-08-03 | 大连理工大学 | A kind of preparation method of high hydrophobicity high temperature resistant fluoresent coating |
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| CN108409911B (en) * | 2018-01-19 | 2020-07-14 | 大连理工大学 | Preparation method of super-hydrophobic self-cleaning fluorescent coating |
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| CN109608689B (en) * | 2018-11-15 | 2021-08-10 | 华南理工大学 | Super-hydrophobic sponge and preparation method and application thereof |
| CN116081623A (en) * | 2023-04-11 | 2023-05-09 | 华侨大学 | Super-hydrophobic activated carbon material and preparation method and application thereof |
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