CN108976667A - The preparation method and product of a kind of super hydrophobic material and application - Google Patents
The preparation method and product of a kind of super hydrophobic material and application Download PDFInfo
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- CN108976667A CN108976667A CN201810904068.0A CN201810904068A CN108976667A CN 108976667 A CN108976667 A CN 108976667A CN 201810904068 A CN201810904068 A CN 201810904068A CN 108976667 A CN108976667 A CN 108976667A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
Abstract
The invention discloses a kind of preparation method of super hydrophobic material and product and application, which includes: to prepare hydrated SiO 2 using sodium metasilicate as raw material；Processing is modified to hydrated SiO 2；Modified hydrated SiO 2, EHP initiator and chloroethylene polymerization are generated into Corvic, Corvic compression molding obtains the super hydrophobic material.The super hydrophobic material has the effect of super-hydrophobic, automatically cleaning scale inhibition, so that super hydrophobic material be applied in industrial pipeline, directly can prevent or reduce calcium sulfate scale from source and deposit in inner wall of the pipe, considerably reduce calcium sulfate scaling bring risk.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to the preparation method and product of a kind of super hydrophobic material and answers
With.
Background technique
Calcium sulfate is a kind of micro-soluble material, since formation heavily fortified point is easily precipitated in the influences such as temperature, pressure, flow velocity in industrial pipeline
Hard calcium sulfate scale body, causes pipeline flow sectional area to become smaller, and causes stress loss, discharge capacity reduction and line clogging；It can also lure
Pipeline local corrosion is sent out, leads to pipe leakage frequently, or even perforation damages sexual behavior event.The mechanism of calcium sulfate scaling includes
Thermodynamics mechanism and kinetics mechanism, when the temperature of solution, pressure, flow velocity change concentrated water will fouling, knot
The rate of dirt is related with temperature and fluid dynamics, and temperature increases or Reynolds number increase can all reduce scaling rate.According to micro-
The solution principle of dissolved salt, when the product of the concentration of sulfate radical and the concentration of calcium ion is greater than the solubility product of calcium sulfate, calcium sulfate is just
Meeting fouling, generates the higher calcium sulfate scale of hardness, and precipitate crystal.The scaling process of calcium sulfate can substantially be divided into following four
Step: the zwitterion in solution interacts to form ion pair；Ion is assembled to form bigger aggregation；Homogeneous nucleation and crystalline substance
Body grows the nucleus to be formed and be not easy in dissolution；Nonhomogen-ous nucleation crystal adsorbs on the contact surface.The form and temperature of calcium sulfate scale
Spend it is related, when temperature be lower than 50 DEG C when form CaSO4·2H2O forms CaSO when temperature is between 50~82 DEG C4·1/
2H2O, when temperature then forms anhydrous CaSO at 82 DEG C or more4, it is also most stable of calcium sulfate, and solubility compares first two
Crystal of calcium sulfate is also minimum, but in most of calcium sulfate scale layers mainly based on calcium sulphate dihydrate.
The control method of calcium sulfate scale has chemical scale inhibition method, physical oil production method, technique antiscale method and physical chemistry at present
Cooperate with antiscale method.Chemical scale inhibition method is to prevent or delay the generation of calcium sulfate using the chemical property of chemical agent itself.
Wherein inhibitor mechanism has following several: (1) chelation: coordinate bond is combined with the ion in solution, and what is worked is scale inhibition
Multiple coordinate bonds on agent molecule form stable complex or solubility by the combination of coordinate bond and effects of ion
Chelate.(2) distortion of lattice acts on: in solution, antisludging agent molecule is relatively adsorbed on the plane of crystal in developmental process, makes
Crystal is distorted.(3) peptizaiton: being acted on by electrostatic repulsion and hinder contacting with each other between microcrystal, avoids crystal poly-
Collection forms bigger crystal.The advantages of chemical scale inhibition agent, is scale inhibition performance height, suitable for acid, alkali or neutrality containing various ions
Solution.The research of chemical scale inhibition method has had the result of comparative maturity.Physical oil production method is by using special physics instrument
Device slows down or prevents the formation of calcium sulfate.Physical oil production technology mainly has seed technology and electricity, magnetosonic etc..Technique antiscale
Method is mainly to reach the method for reducing calcium sulfate scale by changing process conditions；Its core is to change calcium sulfate scaling
Influence factor, to inhibit the generation of calcium sulfate scale.The many because being known as of calcium sulfate scaling are influenced, studies have shown that influence factor
Including temperature, pressure, flow velocity, material and salinity etc.；Experiment shows that the relationship of temperature and calcium sulfate dissolution is not simple
Linear relationship, but first rise to reach most to be worth in a certain temperature and then decline again with the rising of temperature.Therefore technique antiscale
Method makes calcium sulfate dissolution reach maximum generally by suitable temperature is adjusted, and slows down the generation of calcium sulfate scale；Or research
Ion and pH value of solution contained in solution adjust the ion concentration in solution, rationally to reduce the supersaturation of solution calcium sulfate
Degree, slows down calcium sulfate scaling；Or pipe surface is modified using low-surface-energy material, to slow down calcium sulfate in inner wall of the pipe
Deposition.
The descaling method generallyd use at this stage has physical method and chemical method.It is hard that physical method only works as calcium sulfate scale
When, available physical method is shaken, when calcium sulfate is bonded closer with inner wall of the pipe, the effect of physical method
With regard to bad.Chemical scale inhibition method is common method, and scale removal effect is preferable；But chemical cleaning complex process, it expends a large amount of
Chemicals causes production cost to increase, and is unfavorable for large-scale industrial production, and pipeline easy to damage, pollutes environment.
Meanwhile currently to the research of calcium sulfate scale rest on mostly solution containing only sulfate radical or calcium ion or also containing it is a small number of other
In the solution of ion；When in the effluent of institute of factory containing other a large amount of substances, due to will affect scale inhibition between effects of ion
It is difficult to reach scale inhibition effect, therefore the scale inhibition effect of antisludging agent will decline.Many producers' processing calcium sulfate scales still using NaOH or
Na2CO3It impregnates, then removes calcium sulfate scale, but treatment effeciency is low.
Solve the problems, such as calcium sulfate scaling the best way be inhibit fouling, from source control calcium sulfate scale deposition rather than
It is removed again after calcium sulfate is deposited.Chinese patent CN103589067A discloses that " a kind of nanometer with scale effect is multiple
Close plastics and preparation method thereof ", which is by antisludging agent, plasticizer, solubilizer and plastic master batch together melting mixing, makes
The nano composite plastics containing antisludging agent that grain, molding obtain, the antisludging agent on surface can prevent inorganic salt precipitates in plastic table
The adherency in face, to effectively prevent the fouling of frosting.The patent is by adding antisludging agent in the composite to reality
Existing scale inhibition function, since antisludging agent mixes in the composite, so antisludging agent is not necessarily just distributed in composite material
Surface, therefore the patent scale inhibition effect is general.
Therefore the present invention proposes the preparation method and product and application of a kind of super hydrophobic material, is made using the method for the present invention
Super hydrophobic material have super-hydrophobicity, which is used in the production of industrial pipeline, to prevent calcium sulfate scale
Upper deposition, considerably reduces calcium sulfate scaling bring risk in the industrial pipeline.
Summary of the invention
The shortcomings that overcoming the above prior art: the technical problem to be solved by the present invention is to provide a kind of super hydrophobic material
Preparation method and product and application.
Technical solution of the invention is as follows:
The technical solution of the first aspect of the invention is:
A kind of preparation method of super hydrophobic material, comprising the following steps:
(1) sodium silicate solution is mixed with distilled water, is ultrasonically treated 5~15min, is completely dissolved sodium silicate solution；
(2) sodium silicate solution in step (1) is heated, keeping temperature is 35~45 DEG C, and hydrochloric acid is added and carries out instead
It answers, obtains white suspension after the reaction was completed, white suspension is filtered and is precipitated, it is heavy to be washed repeatedly with distilled water
It forms sediment, and uses AgNO3Solution detects the Cl in washing lotion-, generated until being precipitated in washing lotion without AgCl；60~80 DEG C of normal pressure drying are heavy
It forms sediment, hydrated SiO 2 is made；
(3) hydrated SiO 2 in step (2) is mixed with dehydrated alcohol, is slowly added to vinyl triethoxyl silicon
Alkane is uniformly mixed, and adjusts pH to 7~8,35~45 DEG C of constant temperature stir 15~25h, are cooled to room temperature, are centrifuged, true at 55~65 DEG C
Sky is dry, grinds and modified hydrated SiO 2 is made；
(4) stainless steel cauldron is added in hydrated SiO 2 modified in step (3) and deionized water, EHP initiator
It is interior, it is filled with nitrogen discharge air into stainless steel cauldron, is warming up to 55~60 DEG C；
(5) it controls temperature in vinyl chloride monomer storage tank and opens vinyl chloride monomer storage tank lower than temperature in stainless steel cauldron
With the connection of stainless steel cauldron, vinyl chloride monomer is continuously added in stainless steel cauldron with gas phase, and it is anti-to adjust stainless steel
It answers the pressure in kettle to 0.85~0.95MPa, that is, polymerize and Corvic is made；
(6) Corvic in step (5) is pressed and molded, molding temperature is 160~200 DEG C, when molding
Between be 8~12min, obtain super hydrophobic material.
As optimal technical scheme, in the step (1), the mass ratio of sodium silicate solution and distilled water is 1:5, ultrasound
Handle 10min.
As optimal technical scheme, in the step (2), the temperature of sodium silicate solution is kept for 38~42 DEG C；Hydrochloric acid it is dense
Degree is 5mol/L, and hydrochloric acid and sodium silicate solution volume ratio are 0.8~1.2:1.
As optimal technical scheme, in the step (2), the temperature of sodium silicate solution is kept for 40 DEG C；Hydrochloric acid and sodium metasilicate
Liquor capacity ratio is 1:1；Drying temperature is 70 DEG C.
As optimal technical scheme, in the step (3), the anhydrous second of every 1g hydrated SiO 2 and 0.8~1.2ml
Alcohol mixing；The vinyltriethoxysilane of 0.06~0.1ml is added in the hydrated SiO 2 of every 1g；Ammonium hydroxide is added to adjust
PH to 7~8,40 DEG C of degree stir 20h, are dried in vacuo at 60 DEG C.
As optimal technical scheme, in the step (4), the mass ratio of modified hydrated SiO 2 and deionized water is
1:45~55；The mass ratio of modified hydrated SiO 2 and EHP initiator is 1:0.08~0.012, is warming up to 57 DEG C.
As optimal technical scheme, in the step (5), in the step (5), polyvinyl chloride and modified hydration dioxy
The mass ratio of SiClx is 100:3~6, the pressure in adjusting stainless steel cauldron to 0.9MPa.
It is further preferred, in the step (5), in the step (5), polyvinyl chloride and modified hydration titanium dioxide
The mass ratio of silicon is 100:4~5.
As optimal technical scheme, in the step (6), Corvic is particularly put into vulcanizing press
On be pressed and molded, molding temperature be 180 DEG C, clamp time 10min.
The technical solution of the second aspect of the invention is:
Using super hydrophobic material made from above-mentioned preparation method, the contact angle of the super hydrophobic material is greater than 150 °.
The technical solution of the third aspect of the invention is:
Super hydrophobic material obtained above is preparing the application in industrial pipeline.
The beneficial effects of the present invention are:
1, its contact angle is measured by contact angle measurement using super hydrophobic material made from the method for the present invention and is greater than 150 °,
Have the effect of super-hydrophobic, automatically cleaning scale inhibition, so that super hydrophobic material is applied in industrial pipeline, it can be directly from source
It prevents or reduces calcium sulfate scale to deposit in inner wall of the pipe, considerably reduces calcium sulfate scaling bring risk.
2, the method that the present invention uses free radical polymerization；It is organically-modified to hydrated SiO 2 progress simultaneously, pass through control
Modified condition keeps modified hydrated SiO 2 not easy to reunite and energy fine dispersion, to effectively improve polyvinyl chloride
Mechanical property；And pass through the preparation technology parameters such as control polymerization, so that organic inorganic hybridization super hydrophobic material be made, realize certainly
It cleans while preventing calcium sulfate scaling.
3, the present invention prepares super hydrophobic material using the method for organic inorganic hybridization, obtains preferable hydrophobic performance with low cost
Super hydrophobic material, be suitable for large-scale production.
Specific embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Apply example.
Embodiment one
(1) 10g sodium silicate solution is weighed in beaker, 50ml distilled water is added, and is ultrasonically treated 5~15min, is made silicic acid
Sodium solution is completely dissolved；
(2) sodium silicate solution in beaker is heated, keeping temperature is 35 DEG C, and 5mol/L salt is added dropwise into beaker
Acid is reacted, and the volume that is added of hydrochloric acid is 0.8 times of sodium silicate solution volume, until there is white suspension, has been reacted
At white suspension is filtered and is precipitated, washs precipitating repeatedly with distilled water, and use AgNO3Solution detects in washing lotion
Cl-, generated until being precipitated in washing lotion without AgCl；60 DEG C of drying precipitatings of normal pressure, are made hydrated SiO 2；
(3) 100g hydrated SiO 2 obtained above and 80mL dehydrated alcohol are added in 250mL there-necked flask, by 6ml
Vinyltriethoxysilane be slowly added dropwise in three-necked flask be uniformly mixed, be added ammonium hydroxide adjust pH to 7~8,35 DEG C of perseverances
Temperature stirring 15h, is cooled to room temperature, is centrifuged, be dried in vacuo at 55 DEG C, grinds and modified hydrated SiO 2 is made；
(4) be added into the stainless steel cauldron of 100ml the modified hydrated SiO 2 of 1g, 45ml deionized water,
0.08gEHP initiator is filled with nitrogen discharge air into stainless steel cauldron, is warming up to 55 DEG C；
(5) it controls temperature in vinyl chloride monomer storage tank and opens vinyl chloride monomer storage tank lower than temperature in stainless steel cauldron
With the connection of stainless steel cauldron, vinyl chloride monomer is continuously added in stainless steel cauldron with gas phase, and it is anti-to adjust stainless steel
It answers the pressure in kettle to 0.85MPa, that is, polymerize and Corvic is made；Wherein Corvic and modified hydration dioxy
The mass ratio of SiClx is 100:3.
(6) Corvic is put on vulcanizing press and is pressed and molded, molding temperature is 160 DEG C, when molding
Between be 8min, obtain the super hydrophobic material.
Embodiment two
(1) 10g sodium silicate solution is weighed in beaker, 50ml distilled water is added, and is ultrasonically treated 5~15min, is made silicic acid
Sodium solution is completely dissolved；
(2) sodium silicate solution in beaker is heated, keeping temperature is 37 DEG C, and 5mol/L salt is added dropwise into beaker
Acid is reacted, and the volume that is added of hydrochloric acid is 0.9 times of sodium silicate solution volume, until there is white suspension, has been reacted
At white suspension is filtered and is precipitated, washs precipitating repeatedly with distilled water, and use AgNO3Solution detects in washing lotion
Cl-, generated until being precipitated in washing lotion without AgCl；65 DEG C of drying precipitatings of normal pressure, are made hydrated SiO 2；
(3) 100g hydrated SiO 2 obtained above and 90mL dehydrated alcohol are added in 250mL there-necked flask, by 7ml
Vinyltriethoxysilane be slowly added dropwise in three-necked flask be uniformly mixed, be added ammonium hydroxide adjust pH to 7~8,37 DEG C of perseverances
Temperature stirring 17h, is cooled to room temperature, is centrifuged, be dried in vacuo at 60 DEG C, grinds and modified hydrated SiO 2 is made；
(4) be added into the stainless steel cauldron of 100ml the modified hydrated SiO 2 of 1g, 47ml deionized water,
0.09gEHP initiator is filled with nitrogen discharge air into stainless steel cauldron, is warming up to 56 DEG C；
(5) it controls temperature in vinyl chloride monomer storage tank and opens vinyl chloride monomer storage tank lower than temperature in stainless steel cauldron
With the connection of stainless steel cauldron, vinyl chloride monomer is continuously added in stainless steel cauldron with gas phase, and it is anti-to adjust stainless steel
It answers the pressure in kettle to 0.9MPa, that is, polymerize and Corvic is made；Wherein Corvic and modified hydration titanium dioxide
The mass ratio of silicon is 100:4.
(6) Corvic is put on vulcanizing press and is pressed and molded, molding temperature is 170 DEG C, when molding
Between be 10min, obtain the super hydrophobic material.
Embodiment three
(1) 10g sodium silicate solution is weighed in beaker, 50ml distilled water is added, and is ultrasonically treated 5~15min, is made silicic acid
Sodium solution is completely dissolved；
(2) sodium silicate solution in beaker is heated, keeping temperature is 40 DEG C, and 5mol/L salt is added dropwise into beaker
Acid is reacted, and the volume that is added of hydrochloric acid is 1 times of sodium silicate solution volume, until there is white suspension, has been reacted
At white suspension is filtered and is precipitated, washs precipitating repeatedly with distilled water, and use AgNO3Solution detects in washing lotion
Cl-, generated until being precipitated in washing lotion without AgCl；70 DEG C of drying precipitatings of normal pressure, are made hydrated SiO 2；
(3) 100g hydrated SiO 2 obtained above and 100mL dehydrated alcohol are added in 250mL there-necked flask, it will
The vinyltriethoxysilane of 8ml be slowly added dropwise in three-necked flask be uniformly mixed, be added ammonium hydroxide adjust pH to 7~8,40
DEG C constant temperature stirs 20h, is cooled to room temperature, and is centrifuged, and is dried in vacuo at 60 DEG C, grinds and modified hydrated SiO 2 is made；
(4) 1g modified hydrated SiO 2,50ml deionized water, 0.1gEHP are added into the stainless steel cauldron of 100ml
Initiator is filled with nitrogen discharge air into stainless steel cauldron, is warming up to 57 DEG C；
(5) it controls temperature in vinyl chloride monomer storage tank and opens vinyl chloride monomer storage tank lower than temperature in stainless steel cauldron
With the connection of stainless steel cauldron, vinyl chloride monomer is continuously added in stainless steel cauldron with gas phase, and it is anti-to adjust stainless steel
It answers the pressure in kettle to 0.9MPa, that is, polymerize and Corvic is made；Wherein Corvic and modified hydration titanium dioxide
The mass ratio of silicon is 100:4；
(6) Corvic is put on vulcanizing press and is pressed and molded, molding temperature is 180 DEG C, when molding
Between be 10min, obtain the super hydrophobic material.
Example IV
(1) 10g sodium silicate solution is weighed in beaker, 50ml distilled water is added, and is ultrasonically treated 5~15min, is made silicic acid
Sodium solution is completely dissolved；
(2) sodium silicate solution in beaker is heated, keeping temperature is 42 DEG C, and 5mol/L salt is added dropwise into beaker
Acid is reacted, and the volume that is added of hydrochloric acid is 1.1 times of sodium silicate solution volume, until there is white suspension, has been reacted
At white suspension is filtered and is precipitated, washs precipitating repeatedly with distilled water, and use AgNO3Solution detects in washing lotion
Cl-, generated until being precipitated in washing lotion without AgCl；72 DEG C of drying precipitatings of normal pressure, are made hydrated SiO 2；
(3) 100g hydrated SiO 2 obtained above and 110mL dehydrated alcohol are added in 250mL there-necked flask, it will
The vinyltriethoxysilane of 9ml be slowly added dropwise in three-necked flask be uniformly mixed, be added ammonium hydroxide adjust pH to 7~8,35
DEG C constant temperature stirs 22h, is cooled to room temperature, and is centrifuged, and is dried in vacuo at 62 DEG C, grinds and modified hydrated SiO 2 is made；
(4) be added into the stainless steel cauldron of 100ml the modified hydrated SiO 2 of 1g, 52ml deionized water,
0.11gEHP initiator is filled with nitrogen discharge air into stainless steel cauldron, is warming up to 59 DEG C；
(5) it controls temperature in vinyl chloride monomer storage tank and opens vinyl chloride monomer storage tank lower than temperature in stainless steel cauldron
With the connection of stainless steel cauldron, vinyl chloride monomer is continuously added in stainless steel cauldron with gas phase, and it is anti-to adjust stainless steel
It answers the pressure in kettle to 0.95MPa, that is, polymerize and Corvic is made；Wherein Corvic and modified hydration dioxy
The mass ratio of SiClx is 100:5.
(6) Corvic is put on vulcanizing press and is pressed and molded, molding temperature is 190 DEG C, when molding
Between be 11min, obtain the super hydrophobic material.
Embodiment five
(1) 10g sodium silicate solution is weighed in beaker, 50ml distilled water is added, and is ultrasonically treated 5~15min, is made silicic acid
Sodium solution is completely dissolved；
(2) sodium silicate solution in beaker is heated, keeping temperature is 45 DEG C, and 5mol/L salt is added dropwise into beaker
Acid is reacted, and the volume that is added of hydrochloric acid is 1.2 times of sodium silicate solution volume, until there is white suspension, has been reacted
At white suspension is filtered and is precipitated, washs precipitating repeatedly with distilled water, and use AgNO3Solution detects in washing lotion
Cl-, generated until being precipitated in washing lotion without AgCl；75 DEG C of drying precipitatings of normal pressure, are made hydrated SiO 2；
(3) 100g hydrated SiO 2 obtained above and 120mL dehydrated alcohol are added in 250mL there-necked flask, it will
The vinyltriethoxysilane of 10ml be slowly added dropwise in three-necked flask be uniformly mixed, be added ammonium hydroxide adjust pH to 7~8,45
DEG C constant temperature stirs 25h, is cooled to room temperature, and is centrifuged, and is dried in vacuo at 65 DEG C, grinds and modified hydrated SiO 2 is made；
(4) be added into the stainless steel cauldron of 100ml the modified hydrated SiO 2 of 1g, 55ml deionized water,
0.12gEHP initiator is filled with nitrogen discharge air into stainless steel cauldron, is warming up to 60 DEG C；
(5) it controls temperature in vinyl chloride monomer storage tank and opens vinyl chloride monomer storage tank lower than temperature in stainless steel cauldron
With the connection of stainless steel cauldron, vinyl chloride monomer is continuously added in stainless steel cauldron with gas phase, and it is anti-to adjust stainless steel
It answers the pressure in kettle to 0.95MPa, that is, polymerize and Corvic is made；Wherein Corvic and modified hydration dioxy
The mass ratio of SiClx is 100:6.
(6) Corvic is put on vulcanizing press and is pressed and molded, molding temperature is 200 DEG C, when molding
Between be 12min, obtain the super hydrophobic material.
Comparative example one
Remove the step (3) in embodiment one, i.e., hydrated SiO 2 is not modified, other steps and embodiment
One is identical.
Comparative example two
Vinyltriethoxysilane in one step of embodiment (3) is changed to silane coupling agent kh560, and is not ammoniated
Water adjusts pH, other steps are the same as example 1.
Comparative example three
50 DEG C will be warming up in one step of embodiment (4), in step (5) adjust stainless steel cauldron in pressure to
0.5MPa；The mass ratio of Corvic and modified hydrated SiO 2 is 100:1.Other steps are the same as example 1.
Comparative example four
70 DEG C will be warming up in one step of embodiment (4), in step (5) adjust stainless steel cauldron in pressure to
1.5MPa；The mass ratio of Corvic and modified hydrated SiO 2 is 100:10.Other steps and one phase of embodiment
Together.
Super hydrophobic material obtained in embodiment and comparative example is tested, test method is as follows:
(1) the super hydrophobic material water contact angle is measured using contact angle measurement.
(2) it takes a certain amount of water droplet in the super hydrophobic material surface with syringe, observes the state of water droplet.
(3) on the super hydrophobic material surface, paving spills carbon dust as dirt, then water is allowed to flow through, and whether observation carbon dust can be by water
Stream is taken away.
(4) pipeline is made in the production of Mr. Yu industrial enterprise in the super hydrophobic material, material is continued through in pipeline, it should
Ca is mainly contained in material2+、Mg2+、SO42-、Cl-, Ca2+Concentration be 5mol/L, Mg2+Concentration be 2mol/L, SO42-'s
Concentration is 4.5mol/L, Cl-Concentration be 3mol/L, the temperature of material is 35~40 DEG C, and the flow velocity of material is 1~1.2m/s；
Observation 15 days and June after, inner wall of the pipe fouling condition.
Test result is as shown in table 1:
1 super hydrophobic material water contact angle of table and dirt residual condition
Firstly, the water by the super hydrophobic material that it can be seen from the result of method (1) prepared by embodiment one to five in table 1 connects
Feeler has super-hydrophobicity all at 150 ° or more.By in table 1 it can be seen from the result of method (2) water droplet in the super-hydrophobic material
Material surface forms water droplet without drawout, to find out that the super hydrophobic material has super-hydrophobicity.By method in table 1
(3) result can be seen that carbon dust and be taken away by water flow, it is known that the super hydrophobic material has hydrophobic self-cleaning effect.By table
The result of method (4) can be seen that the pipeline prepared by the super hydrophobic material behind 15 days and 6 months in 1, and inner wall does not have
There are dirt deposits, it is known that the material has the function of anti-calcium sulfate scaling.
Secondly, by embodiment as can be seen that super hydrophobic material made from the embodiment of the present invention one to five compared with comparative example
Hydrophobic self-cleaning effect, anti-calcium sulfate scaling effect be apparently higher than comparative example one (hydrated SiO 2 not being modified),
(hydrated SiO 2 additive amount is few and polymeric reaction condition for comparative example two (modified silane coupling agent difference), comparative example three
It is different), comparative example three (hydrated SiO 2 additive amount is more and polymeric reaction condition is different), especially with the effect of embodiment three
Most preferably, it is seen that whether hydrated SiO 2 of the invention be modified, the matter of modified condition and parameter, silica and polyvinyl chloride
Measure the effect that the anti-calcium sulfate scaling of the super hydrophobic material can be all influenced than, polymeric reaction condition and parameter etc..Therefore the present invention adopts
With specific modified condition and the mass ratio of parameter, silica and polyvinyl chloride, polymeric reaction condition, technological parameter etc.,
So that super hydrophobic material obtained is had the effect of anti-calcium sulfate scaling, be used in industrial pipeline, can directly be prevented from source or
It reduces calcium sulfate scale to deposit in inner wall of the pipe, considerably reduces calcium sulfate scaling bring risk.
The above is only feature implementation examples of the invention, are not limited in any way to the scope of the present invention.It is all to use together
The technical solution formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (10)
1. a kind of preparation method of super hydrophobic material, it is characterised in that: the following steps are included:
(1) sodium silicate solution is mixed with distilled water, is ultrasonically treated 5~15min, is completely dissolved sodium silicate solution；
(2) sodium silicate solution in step (1) is heated, keeping temperature is 35~45 DEG C, and hydrochloric acid is added and is reacted, instead
White suspension should be obtained after the completion, white suspension is filtered and is precipitated, precipitating is washed repeatedly with distilled water, is used in combination
AgNO3Solution detects the Cl in washing lotion-, generated until being precipitated in washing lotion without AgCl；60~80 DEG C of drying precipitatings of normal pressure, are made water
Close silica；
(3) hydrated SiO 2 in step (2) is mixed with dehydrated alcohol, is slowly added to vinyltriethoxysilane mixing
Uniformly, pH to 7~8 is adjusted, 35~45 DEG C of constant temperature stir 15~25h, are cooled to room temperature, be centrifuged, are dried in vacuo at 55~65 DEG C,
Modified hydrated SiO 2 is made in grinding；
(4) hydrated SiO 2 modified in step (3) and deionized water, EHP initiator are added in stainless steel cauldron, to not
It is filled with nitrogen discharge air in rust steel reaction kettle, is warming up to 55~60 DEG C；
(5) control in vinyl chloride monomer storage tank temperature lower than temperature in stainless steel cauldron, open vinyl chloride monomer storage tank with not
The connection of rust steel reaction kettle, vinyl chloride monomer are continuously added in stainless steel cauldron with gas phase, adjust stainless steel cauldron
Interior pressure polymerize and Corvic is made to 0.85~0.95MPa；
(6) Corvic in step (5) is pressed and molded, molding temperature is 160~200 DEG C, clamp time 8
~12min, obtains super hydrophobic material.
2. the preparation method of super hydrophobic material according to claim 1, it is characterised in that: in the step (1), sodium metasilicate
The mass ratio of solution and distilled water is 1:5, is ultrasonically treated 10min.
3. the preparation method of super hydrophobic material according to claim 1, it is characterised in that: in the step (2), sodium metasilicate
The temperature of solution is kept for 38~42 DEG C；The concentration of hydrochloric acid is 5mol/L, and hydrochloric acid and sodium silicate solution volume ratio are 0.8~1.2:1；
Drying temperature is 70 DEG C.
4. the preparation method of super hydrophobic material according to claim 1, it is characterised in that: in the step (3), every 1g water
Silica is closed to mix with the dehydrated alcohol of 0.8~1.2ml；The second of 0.06~0.1ml is added in the hydrated SiO 2 of every 1g
Alkenyl triethoxysilane；Ammonium hydroxide is added and adjusts pH to 7~8,40 DEG C of stirring 20h, is dried in vacuo at 60 DEG C.
5. the preparation method of super hydrophobic material according to claim 1, it is characterised in that: in the step (4), modified water
The mass ratio for closing silica and deionized water is 1:45~55；The mass ratio of modified hydrated SiO 2 and EHP initiator is
1:0.08~0.012 is warming up to 57 DEG C.
6. the preparation method of super hydrophobic material according to claim 1, it is characterised in that: in the step (5), polychlorostyrene second
The mass ratio of alkene and modified hydrated SiO 2 is 100:3~6.
7. the preparation method of super hydrophobic material according to claim 6, in the step (5), polyvinyl chloride and modified water
The mass ratio for closing silica is 100:4~5, the pressure in adjusting stainless steel cauldron to 0.9MPa.
8. the preparation method of super hydrophobic material according to claim 1, it is characterised in that: in the step (6), specifically
It is to be put into Corvic on vulcanizing press to be pressed and molded, molding temperature is 180 DEG C, clamp time 10min.
9. super hydrophobic material made from -8 any preparation methods according to claim 1, it is characterised in that: the super-hydrophobic material
The contact angle of material is greater than 150 °.
10. super hydrophobic material according to claim 9 is preparing the application in industrial pipeline.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534601A (en) * | 2018-12-17 | 2019-03-29 | 南通寰宇博新化工环保科技有限公司 | A kind of biochemical method for combining electrocatalytic oxidation processing landfill leachate |
| CN112940568A (en) * | 2021-04-14 | 2021-06-11 | 江西省萍乡市富源瓷业有限公司 | Column type composite insulator |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3915922A (en) * | 1972-03-25 | 1975-10-28 | Kanegafuchi Chemical Ind | Polyvinyl chloride composition |
| US20080194736A1 (en) * | 2007-02-13 | 2008-08-14 | Minqiu Lu | PVC nanocomposite manufacturing technology and applications |
| CN101475672A (en) * | 2009-01-14 | 2009-07-08 | 河南大学 | Method for modifying polychloroethylene by in-situ polymerization of nano silicon dioxide |
| CN102199259A (en) * | 2011-04-07 | 2011-09-28 | 安徽大学 | Nano modified chlorinated polyether resin with core-shell structure and preparation method thereof |
| CN102952357A (en) * | 2012-11-29 | 2013-03-06 | 江苏亨通线缆科技有限公司 | Waterproof and flame-retarded PVC (polyvinyl chloride) cable material for data cable and preparation method thereof |
| CN105315801A (en) * | 2015-11-06 | 2016-02-10 | 河南大学 | Preparation method of SiO2/polymer combined superhydrophobic coating |
-
2018
- 2018-08-09 CN CN201810904068.0A patent/CN108976667B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3915922A (en) * | 1972-03-25 | 1975-10-28 | Kanegafuchi Chemical Ind | Polyvinyl chloride composition |
| US20080194736A1 (en) * | 2007-02-13 | 2008-08-14 | Minqiu Lu | PVC nanocomposite manufacturing technology and applications |
| CN101475672A (en) * | 2009-01-14 | 2009-07-08 | 河南大学 | Method for modifying polychloroethylene by in-situ polymerization of nano silicon dioxide |
| CN102199259A (en) * | 2011-04-07 | 2011-09-28 | 安徽大学 | Nano modified chlorinated polyether resin with core-shell structure and preparation method thereof |
| CN102952357A (en) * | 2012-11-29 | 2013-03-06 | 江苏亨通线缆科技有限公司 | Waterproof and flame-retarded PVC (polyvinyl chloride) cable material for data cable and preparation method thereof |
| CN105315801A (en) * | 2015-11-06 | 2016-02-10 | 河南大学 | Preparation method of SiO2/polymer combined superhydrophobic coating |
Non-Patent Citations (3)
| Title |
|---|
| AHMAD ASADINEZHAD: "Recent Progress in Surface Modification of Polyvinyl Chloride", 《MATERIALS》 * |
| 杨洪兴等: "《绿色建筑发展与可再生能源应用》", 31 December 2016, 中国铁道出版社 * |
| 田爱娟: "表面改性纳米SiO2原位聚合增强PVC树脂性能研究", 《中国氯碱》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109534601A (en) * | 2018-12-17 | 2019-03-29 | 南通寰宇博新化工环保科技有限公司 | A kind of biochemical method for combining electrocatalytic oxidation processing landfill leachate |
| CN112940568A (en) * | 2021-04-14 | 2021-06-11 | 江西省萍乡市富源瓷业有限公司 | Column type composite insulator |
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