CN109437780A - A kind of super-hydrophobic automatic cleaning recycled cement and preparation method thereof - Google Patents
A kind of super-hydrophobic automatic cleaning recycled cement and preparation method thereof Download PDFInfo
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- CN109437780A CN109437780A CN201811390892.5A CN201811390892A CN109437780A CN 109437780 A CN109437780 A CN 109437780A CN 201811390892 A CN201811390892 A CN 201811390892A CN 109437780 A CN109437780 A CN 109437780A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/06—Aluminous cements
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1018—Coating or impregnating with organic materials
- C04B20/1029—Macromolecular compounds
- C04B20/1048—Polysaccharides, e.g. cellulose, or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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- Inorganic Chemistry (AREA)
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Abstract
The present invention relates to a kind of super-hydrophobic automatic cleaning recycled cements, and by weight, preparing raw material includes: 100 parts of high alumina cement, 10-30 parts of hydrophobic polymer based on polytetrafluoroethylene (PTFE).The invention further relates to the preparation methods of the super-hydrophobic automatic cleaning recycled cement.Super-hydrophobic automatic cleaning recycled cement self-cleaning performance of the invention is good, hydrophobicity is strong and intensity is high, good market prospect.
Description
Technical field
The present invention relates to hydrophobic technical field of membrane, in particular to a kind of super-hydrophobic automatic cleaning recycled cement and its preparation side
Method.
Background technique
Cement base exterior wall, bridge spanning the sea, sea port dock and steamer etc. are required to largely use cement, are especially applied to
When the special dimensions such as cesspool, soda acid liquid liquid storage tank, it is desirable that cement has better durability.It is generally believed that water body can be by
Gradually corrode cement, so that its intensity be caused to decline, if the hydrophobicity of cement can be improved, can greatly improve cement uses the longevity
Life.
Polytetrafluoroethylene film has the advantages that chemical stability is good and corrosion resistant, can be widely applied to different necks
Domain, especially as the membrane material (super hydrophobic material) of strong-hydrophobicity.The surface of super-hydrophobic polytetrafluoroethylene film typically refer to
The contact angle of water is greater than 150 ° of surface, when water droplet is contacted and rolled with super hydrophobic surface, it will takes away and is attached to admittedly
The pollutant in body surface face, to have self-cleaning ability.
If polytetrafluoroethylene film can be combined with cement, it is likely that obtain that self-cleaning performance is good and very hydrophobic it is new
Type cement.
Summary of the invention
The invention discloses a kind of super-hydrophobic automatic cleaning recycled cements, and by weight, preparing raw material includes:
100 parts of high alumina cement
10-30 parts of hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, by weight, the raw material for preparing of the hydrophobic polymer based on polytetrafluoroethylene (PTFE) includes:
Polytetrafluoroethylene (PTFE) 100
Polysiloxanes 20-50
Polymer modification nanofiller 10-20
Lubricant 5-15
Hydroxypropyl starch ether 5-10
KH-550 1-5
Solvent 60-80.
Preferably, the raw material for preparing of the hydrophobic polymer based on polytetrafluoroethylene (PTFE) includes:
Polytetrafluoroethylene (PTFE) 100
Polysiloxanes 30-40
Polymer modification nanofiller 15-20
Lubricant 10-15
Hydroxypropyl starch ether 6-9
KH-550 2-4
Solvent 70-80.
It is highly preferred that the raw material for preparing of the hydrophobic polymer based on polytetrafluoroethylene (PTFE) includes:
Polytetrafluoroethylene (PTFE) 100
Polysiloxanes 36
Polymer modification nanofiller 17
Lubricant 12
Hydroxypropyl starch ether 7
KH-550 3
Solvent 75.
Preferably, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides and 0.2 gram of tetramethylammonium hydroxide are added in reactor, lead to nitrogen
Protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain polysiloxanes.
Preferably, the polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Preferably, the lubricant is aviation kerosine.
Preferably, the solvent be selected from dimethyl sulfoxide, n,N-Dimethylformamide, n,N-dimethylacetamide, acetone,
At least one of ethyl alcohol, isopropanol；The preferably mixture of n,N-Dimethylformamide and isopropanol；More preferably N, N- bis-
The mixture of methylformamide and isopropanol by weight 1:3.
Preferably, the hydrophobic polymer based on polytetrafluoroethylene (PTFE) prepares raw material further include:
Seven fluorine bytyry imidazoles 1-10 of N-
1,7- dibromo-heptane 1-10.
In one embodiment, the preparation method of the hydrophobic polymer based on polytetrafluoroethylene (PTFE), comprising the following steps:
(1) raw material for preparing the hydrophobic polymer based on polytetrafluoroethylene (PTFE) is stirred and is sufficiently mixed in blender,
To form mixed material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE).
The present invention also provides the methods of super-hydrophobic automatic cleaning recycled cement, comprising the following steps:
After high alumina cement and the hydrophobic polymer based on polytetrafluoroethylene (PTFE) are sufficiently mixed, obtain.
The advantageous effects of invention are as follows:
1, by polymer overmold filler, obtain better dispersion effect, and improve the degree of cross linking with obtain better adhesion strength with
And hydrophobic effect；
2, by the cooperation of different-grain diameter filler, better microstructure is obtained, to improve hydrophobicity；
3, the intensity of system can be improved in the addition of low sulfonation degree graphene oxide；
4, better system dispersibility can be obtained by the adjustment of solvent and improves hydrophobic effect；
5, seven fluorine bytyry imidazoles of N- and 1, the degree of cross linking of film can be improved in 7- dibromo-heptane, to improve intensity.
Specific embodiment
Raw material:
Sulfoxidation graphene the preparation method comprises the following steps:
By weight, 1 part of graphene oxide, 10 parts of chloroethyl sodium sulfonate, 6 parts of potassium hydroxide and 300 parts of deionized water are added
Enter in reactor, after 3 parts of concentrated nitric acid is then added and is warming up to 50 DEG C of reactions 1-5 hours, reaction solution is poured into ice water, ice is used
After water washing obtained solid 3 times, by the sulfoxidation graphene of sufficiently dry the different sulfonation degrees of the solid；
Specifically, the reaction time is 1 hour, obtains the graphene oxide that sulfonation degree is about 10% and obtains when the reaction time is 5 hours
Obtain the graphene oxide that sulfonation degree is about 30%.
Other raw materials are commercially available.
Embodiment 1
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 20 grams of polysiloxanes, 10 grams of polymer modification nanofiller, 5 grams of aviation kerosine, hydroxypropyl
5 grams of base starch ether, 1 gram of KH-550,60 grams of solvent (mixture of n,N-Dimethylformamide and isopropanol by weight 1:3)
It stirs and is sufficiently mixed in blender, to form mixed material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reaction is added in basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide
In device, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon
Oxygen alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Embodiment 2
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 30 grams of polysiloxanes, 15 grams of polymer modification nanofiller, 10 grams of aviation kerosine, hydroxyl
6 grams of propyl starch ether, 2 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 70 grams of solvent
Object) it stirs and is sufficiently mixed in blender, to form mixed material, then it is small to stand curing 5 at normal temperature for the mixed material
When；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reaction is added in basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide
In device, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon
Oxygen alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Embodiment 3
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 36 grams of polysiloxanes, 17 grams of polymer modification nanofiller, 12 grams of aviation kerosine, hydroxyl
7 grams of propyl starch ether, 3 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 75 grams of solvent
Object) it stirs and is sufficiently mixed in blender, to form mixed material, then it is small to stand curing 5 at normal temperature for the mixed material
When；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reaction is added in basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide
In device, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon
Oxygen alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Embodiment 4
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 36 grams of polysiloxanes, 17 grams of polymer modification nanofiller, 12 grams of aviation kerosine, hydroxyl
7 grams of propyl starch ether, 3 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 75 grams of solvent
Object), seven 5 grams of fluorine bytyry imidazoles of N-, 5 grams of 1,7- dibromo-heptane stir and be sufficiently mixed in blender, to form mixture
Material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reaction is added in basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide
In device, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon
Oxygen alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Comparative example 1
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 36 grams of polysiloxanes, 17 grams of polymer modification nanofiller, 12 grams of aviation kerosine, hydroxyl
7 grams of propyl starch ether, 3 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 75 grams of solvent
Object), seven 5 grams of fluorine bytyry imidazoles of N-, 5 grams of 1,7- dibromo-heptane stir and be sufficiently mixed in blender, to form mixture
Material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reactor is added in basic ring tetrasiloxane, 5 grams of sulfoxidation graphenes (sulfonation degree 30%) and 0.2 gram of tetramethylammonium hydroxide
In, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon oxygen
Alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Comparative example 2
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 36 grams of polysiloxanes, 17 grams of polymer modification nanofiller, 12 grams of aviation kerosine, hydroxyl
7 grams of propyl starch ether, 3 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 75 grams of solvent
Object), seven 5 grams of fluorine bytyry imidazoles of N-, 5 grams of 1,7- dibromo-heptane stir and be sufficiently mixed in blender, to form mixture
Material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reaction is added in basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide
In device, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon
Oxygen alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) reactor is added in 2 mol of 1,2- propylene glycol, trimethylolpropane 0.5 mol and Mono-n-butyltin 0.01mol
In, after argon gas is protected and is warming up to 90 DEG C of reactions 2 hours, then it is warming up to 270 DEG C and vacuum degree is adjusted to less than 0.02 megapascal
Afterwards, after the reaction was continued 6 hours, it is cooled to room temperature, then n,N-Dimethylformamide 1000ml, β-ring paste is added into reactor
Smart 0.2mol and silane coupling agent KH-560 0.05mol, after then heating to 110 DEG C of reactions 10 hours, by reaction solution
It is poured into water, it is after being washed with water obtained solid 3 times, the solid is sufficiently dry, obtain cyclo-dextrin-modified polyester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Comparative example 3
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 36 grams of polysiloxanes, 17 grams of polymer modification nanofiller, 12 grams of aviation kerosine, hydroxyl
7 grams of propyl starch ether, 3 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 75 grams of solvent
Object), seven 5 grams of fluorine bytyry imidazoles of N-, 5 grams of 1,7- dibromo-heptane stir and be sufficiently mixed in blender, to form mixture
Material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 85 grams of 1,3,5,7- tetramethyl-ring tetrasiloxanes, 5 grams of low sulfonation degree oxygen
Graphite alkene (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide are added in reactor, lead to nitrogen protection, stir and heat up
To 90 DEG C react 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain polysiloxanes；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
Comparative example 4
By weight, in blender, by 100 parts of high alumina cement and 20 parts of the hydrophobic polymer based on polytetrafluoroethylene (PTFE)
After being sufficiently mixed, super-hydrophobic automatic cleaning recycled cement is obtained；
The hydrophobic polymer based on polytetrafluoroethylene (PTFE) the preparation method comprises the following steps:
(1) by 100 grams of polytetrafluoroethylene (PTFE), 36 grams of polysiloxanes, 17 grams of polymer modification nanofiller, 12 grams of aviation kerosine, hydroxyl
7 grams of propyl starch ether, 3 grams of the KH-550, (mixing of n,N-Dimethylformamide and isopropanol by weight 1:3 of 75 grams of solvent
Object), seven 5 grams of fluorine bytyry imidazoles of N-, 5 grams of 1,7- dibromo-heptane stir and be sufficiently mixed in blender, to form mixture
Material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, the polysiloxanes the preparation method comprises the following steps:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Reaction is added in basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides (sulfonation degree 10%) and 0.2 gram of tetramethylammonium hydroxide
In device, lead to nitrogen protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain poly- silicon
Oxygen alkane；
The polymer modification nanofiller the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 5 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 5 grams of hydroxyapatite (1 micron of average grain diameter) and 5 grams of silane coupling agent KH-
550, after maintenance is stirred at room temperature 2 hours, filters and obtained solid is sufficiently dry, obtain polymer modification nanofiller.
Test
By the resulting recycled cement of any one of above-described embodiment 1-4 and comparative example 1-4, fine sand, water according to mass ratio 1:1.5:3
Mixing, stirring form cement slurry；Then cement slurry is poured into mold, super-hydrophobic concrete is obtained after natural air drying.
The performance for testing above-mentioned concrete, as a result see the table below 1.
Table 1
| Example | Water contact angle ° | Roll angle ° |
| Embodiment 1 | 144 | 4 |
| Embodiment 2 | 146 | 4 |
| Embodiment 3 | 157 | 3 |
| Embodiment 4 | 155 | 3 |
| Comparative example 1 | 130 | 6 |
| Comparative example 2 | 132 | 6 |
| Comparative example 3 | 136 | 5 |
| Comparative example 4 | 135 | 5 |
| Pure high alumina cement | 125 | 13 |
Claims (10)
1. a kind of super-hydrophobic automatic cleaning recycled cement, which is characterized in that by weight, preparing raw material includes:
100 parts of high alumina cement
10-30 parts of hydrophobic polymer based on polytetrafluoroethylene (PTFE)；
Wherein, by weight, the raw material for preparing of the hydrophobic polymer based on polytetrafluoroethylene (PTFE) includes:
Polytetrafluoroethylene (PTFE) 100
Polysiloxanes 20-50
Polymer modification nanofiller 10-20
Lubricant 5-15
Hydroxypropyl starch ether 5-10
KH-550 1-5
Solvent 60-80.
2. super-hydrophobic automatic cleaning recycled cement according to claim 1, which is characterized in that by weight, described to be based on
The raw material for preparing of the hydrophobic polymer of polytetrafluoroethylene (PTFE) includes:
Polytetrafluoroethylene (PTFE) 100
Polysiloxanes 30-40
Polymer modification nanofiller 15-20
Lubricant 10-15
Hydroxypropyl starch ether 6-9
KH-550 2-4
Solvent 70-80.
3. super-hydrophobic automatic cleaning recycled cement according to claim 2, which is characterized in that by weight, described to be based on
The raw material for preparing of the hydrophobic polymer of polytetrafluoroethylene (PTFE) includes:
Polytetrafluoroethylene (PTFE) 100
Polysiloxanes 36
Polymer modification nanofiller 17
Lubricant 12
Hydroxypropyl starch ether 7
KH-550 3
Solvent 75.
4. super-hydrophobic automatic cleaning recycled cement according to claim 1, which is characterized in that the preparation side of the polysiloxanes
Method are as follows:
By 10 grams of 3- aminopropyltriethoxy dimethoxysilanes, 30 grams of perfluoro capryl triethoxysilanes, 55 grams of 1,3,5,7- tetramethyls
Basic ring tetrasiloxane, 5 grams of low sulfonation degree graphene oxides and 0.2 gram of tetramethylammonium hydroxide are added in reactor, lead to nitrogen
Protection, stir and be warming up to 90 DEG C reaction 2 hours after, then be warming up to 120 DEG C reaction 1 hour after, obtain polysiloxanes.
5. super-hydrophobic automatic cleaning recycled cement according to claim 1, which is characterized in that the polymer modification nanometer is filled out
Material the preparation method comprises the following steps:
(1) by 1 mol of 1,2- propylene glycol, 1 mol of terephthalic acid (TPA), 0.5 mol of trimethylolpropane and Mono-n-butyltin
0.01mol is added in reactor, argon gas protect and be warming up to 90 DEG C react 2 hours after, then be warming up to 270 DEG C and by vacuum degree tune
Section is after the reaction was continued 6 hours, is cooled to room temperature, then N is added into reactor, N- dimethyl formyl after less than 0.02 megapascal
It is small to then heat to 110 DEG C of reactions 10 by amine 1000ml, beta-cyclodextrin 0.2mol and silane coupling agent KH-560 0.05mol
Reaction solution is poured into water by Shi Hou, after being washed with water obtained solid 3 times, the solid is sufficiently dry, and it is poly- to obtain cyclo-dextrin-modified
Ester；
(2) at room temperature, 20 grams of above-mentioned cyclo-dextrin-modified polyester are dissolved in the DMF of 1000ml, 2 grams of nano oxygen is then added
Change yttrium (300 nanometers of average grain diameter), 3 grams of nano silica (100 nanometers of average grain diameter), 5 grams of hydroxyapatite (averagely
1 micron of partial size) and 5 grams of silane resin acceptor kh-550, after maintenance is stirred at room temperature 2 hours, filter simultaneously that obtained solid is abundant
It is dry, obtain polymer modification nanofiller.
6. super-hydrophobic automatic cleaning recycled cement according to claim 1, which is characterized in that the lubricant is aviation coal
Oil.
7. super-hydrophobic automatic cleaning recycled cement according to claim 1, which is characterized in that it is sub- that the solvent is selected from dimethyl
At least one of sulfone, n,N-Dimethylformamide, n,N-dimethylacetamide, acetone, ethyl alcohol, isopropanol；Preferably N, N-
The mixture of dimethylformamide and isopropanol；More preferably n,N-Dimethylformamide and isopropanol are by weight the mixed of 1:3
Close object.
8. super-hydrophobic automatic cleaning recycled cement according to claim 1, which is characterized in that by weight, described to be based on
The hydrophobic polymer of polytetrafluoroethylene (PTFE) prepares raw material further include:
Seven fluorine bytyry imidazoles 1-10 of N-
1,7- dibromo-heptane 1-10.
9. the preparation method of the hydrophobic polymer based on polytetrafluoroethylene (PTFE), which comprises the following steps:
(1) raw material of the hydrophobic polymer described in the preparation of any one of claim 1-8 based on polytetrafluoroethylene (PTFE) is being stirred
It mixes and stirs and be sufficiently mixed in device, to form mixed material, then the mixed material stands curing 5 hours at normal temperature；
(2) at 60 DEG C, said mixture material is rolled into base band with calender；
(3) it at 150 DEG C, with spoke machine is expanded by after 2 times of above-mentioned base band elder generation longitudinal stretching, then 2 times of cross directional stretch, is sintered in 330 DEG C
Thermal finalization, sintering time are 2 hours, obtain hydrophobic composite membrane material；
(4) the hydrophobic composite membrane material is ground into fine grained, obtains the hydrophobic polymer based on polytetrafluoroethylene (PTFE).
10. the method for super-hydrophobic automatic cleaning recycled cement, which comprises the following steps:
High alumina cement and the described in any item hydrophobic polymers based on polytetrafluoroethylene (PTFE) of claim 1-9 are sufficiently mixed
Afterwards, it obtains.
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