CN112250367A - High-impermeability geopolymer and preparation method thereof - Google Patents
High-impermeability geopolymer and preparation method thereof Download PDFInfo
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- 229920000876 geopolymer Polymers 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 49
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 22
- 239000003513 alkali Substances 0.000 claims abstract description 22
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002131 composite material Substances 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- 239000012190 activator Substances 0.000 claims abstract description 15
- 239000002893 slag Substances 0.000 claims abstract description 14
- 239000006004 Quartz sand Substances 0.000 claims abstract description 12
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 35
- 239000011259 mixed solution Substances 0.000 claims description 24
- 239000000203 mixture Substances 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 10
- 229910017604 nitric acid Inorganic materials 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 10
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- 229910052681 coesite Inorganic materials 0.000 claims description 6
- 229910052906 cristobalite Inorganic materials 0.000 claims description 6
- 229910052682 stishovite Inorganic materials 0.000 claims description 6
- 229910052905 tridymite Inorganic materials 0.000 claims description 6
- 230000032683 aging Effects 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 229910052622 kaolinite Inorganic materials 0.000 claims description 5
- 230000010355 oscillation Effects 0.000 claims description 5
- 235000019353 potassium silicate Nutrition 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 5
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 239000002002 slurry Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 239000000463 material Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 230000005284 excitation Effects 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910000323 aluminium silicate Inorganic materials 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000004927 clay Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052593 corundum Inorganic materials 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical group O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000002440 industrial waste Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910001845 yogo sapphire Inorganic materials 0.000 description 2
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C04B28/006—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 mineral polymers, e.g. geopolymers of the Davidovits type
-
- 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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/04—Alkali metal or ammonium silicate cements ; Alkyl silicate cements; Silica sol cements; Soluble silicate 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
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00293—Materials impermeable to liquids
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/23—Acid resistance, e.g. against acid air or rain
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/76—Use at unusual temperatures, e.g. sub-zero
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a high-impermeability geopolymer which comprises the following components in parts by weight: 37-44 parts of granulated blast furnace slag, 10-20 parts of calcined kaolin, 33-40 parts of quartz sand, 10-12 parts of a composite alkali activator, 9-12 parts of water, 0.05-0.06 part of a dispersing agent, 0.06-0.08 part of a defoaming agent, 1-3 parts of a silane coupling agent and 0.06-0.08 part of a modified multi-walled carbon nanotube. The preparation method of the high-impermeability geopolymer is simple, adopts normal-temperature curing and is easy to popularize. The maximum permeation resistance pressure of the prepared high-permeability-resistant geopolymer reaches more than 5.4MPa, the national standard JC/T984-2011 is that the permeation resistance pressure is more than or equal to 1.5MPa after 28d, and the permeation resistance pressure of the high-permeability-resistant geopolymer is far beyond the industrial standard.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a high-impermeability geopolymer and a preparation method thereof.
Background
The geopolymer is an aluminosilicate cementing material which is formed by reacting an aluminosilicate material with an alkali activator and has an amorphous three-dimensional network structure synthesized by silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron, and belongs to inorganic polymers. At present, a great deal of research is carried out at home and abroad aiming at improving the impermeability of geopolymers, wherein the pore structure of a matrix is improved and optimized mainly by adopting the filling effect of inorganic substances such as glass beads, floating beads, rubber powder and the like. However, with the addition of such inorganic substances, the geopolymer has far from meeting the requirements of social development in terms of strength, durability and water resistance, and further research and improvement are required.
Disclosure of Invention
The invention aims to provide a geopolymer with high impermeability and a preparation method thereof, and the geopolymer material has outstanding high impermeability, high compressive strength, short setting time, good crack resistance and good durability.
The polymer with high impermeability comprises the following components in parts by weight:
37-44 parts of granulated blast furnace slag, 10-20 parts of calcined kaolin, 33-40 parts of quartz sand, 10-12 parts of a composite alkali activator, 9-12 parts of water, 0.05-0.06 part of a dispersing agent, 0.06-0.08 part of a defoaming agent, 1-3 parts of a silane coupling agent and 0.06-0.08 part of a modified multi-walled carbon nanotube.
According to the above scheme, the granulated blast furnace slag contains 30-50 wt% of CaO and SiO2The content is 30-40 wt%, and the particle size is 2000-3000 meshes.
According to the above scheme, the calcined kaolin is prepared in the following manner:
calcining kaolinite at 900 deg.C for 5-6 hr, grinding, sieving to make its grain size less than 200nm and Al content less than2O330-45 wt% of SiO2Is 30-35 wt%.
According to the scheme, the particle size of the quartz sand is 40-80 meshes.
According to the scheme, the composite alkali activator is prepared in the following way:
preparing water glass solution with initial modulus of 3.2-3.4 and solid content of 26-32%, adding solid sodium hydroxide of different quality to obtain sodium water glass with modulus of 1.6-1.8, and aging for 6-11 h.
According to the scheme, the silane coupling agent is any one or mixture of KH550, KH560 and KH 570.
According to the scheme, the modified multi-walled carbon nanotube is prepared in the following way:
placing the multi-walled carbon nano-tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and fully stirring; wherein the mass ratio of the multi-wall carbon nano-tube to the mixed solution is 1/100-1/200, and the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1/2-1/4;
standing after ultrasonic oscillation for 3-6 hours at 40-60 ℃, then diluting with deionized water, and performing centrifugal separation to obtain a precipitate; repeating the dilution, separation and precipitation until the pH of the resulting solution is greater than 7;
drying the obtained solution at 60-70 ℃ in a vacuum environment of 20-30Pa to obtain a preliminarily modified multi-walled carbon nanotube;
adding the preliminarily modified multi-walled carbon nano-tube into a thionyl chloride solvent according to the mass ratio of 1:200, dropwise adding 5 drops of N, N-dimethylformamide as a catalyst, carrying out ultrasonic treatment for 0.5-0.7 h under the power of 300-500W, and then refluxing for 12-20 h under the condition of 60-75 ℃ to obtain the modified multi-walled carbon nano-tube.
The preparation method of the polymer with high impermeability comprises the following steps:
placing the defoaming agent, the dispersing agent, the multi-walled carbon nano tube and the water in the composite alkali-activated solution, stirring for 120-800 s, and then placing under the power of 600-800W for ultrasonic treatment for 0.8-0.9h to obtain a uniform mixed solution;
putting the granulated blast furnace slag, the calcined kaolin and the quartz sand into a stirring pot, and stirring for 60-100s to obtain a mixture;
adding the obtained mixed solution into the obtained mixture, stirring for 90-120s to obtain geopolymer slurry, adding a silane coupling agent, stirring for 90-120s, pouring, vibrating, and curing under standard curing conditions for 28 days to obtain the geopolymer with high impermeability.
Compared with the traditional geopolymer material, the geopolymer with high impermeability has the following main advantages:
1. the high-impermeability geopolymer material adopts industrial wastes such as granulated blast furnace slag, calcined kaolin and the like, can effectively solve the problem of industrial waste stacking, changes waste into valuable, saves the environment and protects the environment;
2. the high-impermeability geopolymer provided by the invention has good crack resistance, even though micro cracks are inevitably generated due to shrinkage of the geopolymer, the silane coupling agent can form a hydrophobic layer in capillary pores and the micro cracks due to excellent hydrophobicity, so that the moisture is prevented from entering and external protection is formed, and a proper amount of moisture and the silane coupling agent in the invention can form a three-dimensional network structure through hydrolysis and polycondensation reaction, so that the effect of enhancing a modified geopolymer matrix is achieved;
3. the common geopolymer has seepage pressure less than 1MP, and the modified geopolymer has stuffing effect, volcanic ash effect and nanometer nucleation effect of modified multiwall carbon nanotube to improve the structure, reduce communication holes, optimize hole structure and reduce porosity. The maximum permeation resistance pressure of the prepared high-permeability-resistant geopolymer reaches more than 5.4MPa, the national standard-JC/T984-2011 standard in China is that the permeation resistance pressure is more than or equal to 1.5MPa after 28d, and the high-permeability-resistant geopolymer is qualified, and the permeation resistance pressure of the high-permeability-resistant geopolymer far exceeds the industrial standard.
4. The preparation method of the high-impermeability geopolymer is simple, adopts normal-temperature curing and is easy to popularize.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The raw materials used in the following examples:
the granulated blast furnace slag contains 30 to 50 weight percent of CaO and SiO2The content is 30-40 wt%, and the particle size is 2000-3000 meshes. The grain size of the quartz sand is 40-80 meshes. The silane coupling agent is any one or mixture of KH550, KH560 and KH 570.
The composite alkali activator is prepared by the following steps:
preparing water glass solution with initial modulus of 3.2-3.4 and solid content of 26-32%, adding solid sodium hydroxide of different quality to obtain sodium water glass with modulus of 1.6-1.8, and aging for 6-11 h.
Calcined kaolin was prepared as follows:
calcining kaolinite at 900 deg.C for 5-6 hr, grinding, sieving to make its grain size less than 200nm and Al content less than2O330-45 wt% of SiO2Is 30-35 wt%.
The modified multi-wall carbon nano-tube is prepared by the following steps:
placing the multi-walled carbon nano-tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and fully stirring; wherein the mass ratio of the multi-wall carbon nano-tube to the mixed solution is 1/100-1/200, and the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1/2-1/4;
standing after ultrasonic oscillation for 3-6 hours at 40-60 ℃, then diluting with deionized water, and performing centrifugal separation to obtain a precipitate; repeating the dilution, separation and precipitation until the pH of the resulting solution is greater than 7;
drying the obtained solution at 60-70 ℃ in a vacuum environment of 20-30Pa to obtain a preliminarily modified multi-walled carbon nanotube;
adding the preliminarily modified multi-walled carbon nano-tube into a thionyl chloride solvent according to the mass ratio of 1:200, dropwise adding 5 drops of N, N-dimethylformamide as a catalyst, carrying out ultrasonic treatment for 0.5-0.7 h under the power of 300-500W, and then refluxing for 12-20 h under the condition of 60-75 ℃ to obtain the modified multi-walled carbon nano-tube.
Example 1
Compound alkali activator: a water glass solution having an initial modulus of 3.2 and a solid content of 32% was prepared, and sodium water glass having a modulus of 1.8 was prepared by adding solid sodium hydroxide thereto, followed by aging for 11 hours.
Calcined kaolin clay: the kaolinite is calcined at 900 ℃ for 5 hours, then ground and sieved, so that the particle size is less than 200nm, 45 wt% of Al2O3 and 30 wt% of SiO 2.
Modified multi-walled carbon nanotubes: placing the multi-walled carbon nano-tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and fully stirring; wherein the mass ratio of the multi-wall carbon nano-tube to the mixed solution is 1/100, and the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1/2; standing after ultrasonic oscillation for 3 hours at 40 ℃, diluting with deionized water, and performing centrifugal separation to obtain a precipitate; repeating the dilution, separation and precipitation until the pH of the resulting solution is greater than 7; drying the obtained solution at 70 ℃ in a vacuum environment of 20 ℃ to obtain a preliminarily modified multi-walled carbon nanotube; adding the preliminarily modified multi-walled carbon nano-tube into a thionyl chloride solvent according to the mass ratio of 1:200, dropwise adding 5 drops of N, N-dimethylformamide as a catalyst, carrying out ultrasonic treatment for 0.5 hour under the power of 500W, and then refluxing for 12 hours at the temperature of 75 ℃ to obtain the modified multi-walled carbon nano-tube.
Pouring 40 parts of granulated blast furnace slag, 15 parts of calcined kaolin and 35 parts of quartz sand which are weighed into a stirrer, stirring for 120s to obtain a mixture, then placing 0.05 part of dispersing agent, 0.06 part of defoaming agent, 0.07 part of modified multi-walled carbon nano tube and 9 parts of water into 12 parts of composite alkali excitation solution, stirring for 120s, placing the mixture into 800W power, carrying out ultrasonic treatment for 0.5 hour to obtain uniform mixed solution, then adding the uniform mixed solution into the mixture, stirring for 100s, finally adding 1 part of silane coupling agent, stirring for 100s, then pouring, vibrating, and curing for 28d under the normal-temperature curing condition to obtain the high-impermeability geopolymer.
Comparative example 1
Comparative example the implementation was carried out as in example 1, but the preparation of the geopolymer was carried out using unmodified multi-walled carbon nanotubes instead of modified multi-walled carbon nanotubes.
Example 2
Compound alkali activator: a water glass solution having an initial modulus of 3.3 and a solid content of 28% was prepared, and sodium water glass having a modulus of 1.8 was prepared by adding solid sodium hydroxide thereto, followed by aging for 11 hours.
Calcined kaolin clay: the kaolinite is calcined at 900 ℃ for 6 hours, then ground and sieved, so that the particle size is less than 200nm, 45 wt% of Al2O3 and 30 wt% of SiO 2.
Modified multi-walled carbon nanotubes: placing the multi-walled carbon nano-tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and fully stirring; wherein the mass ratio of the multi-wall carbon nano-tube to the mixed solution is 1/200, and the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1/2; standing after ultrasonic oscillation for 5 hours at 60 ℃, then diluting with deionized water, and performing centrifugal separation to obtain a precipitate; repeating the dilution, separation and precipitation until the pH of the resulting solution is greater than 7; drying the obtained solution at 70 ℃ in a vacuum environment of 20 ℃ to obtain a preliminarily modified multi-walled carbon nanotube; adding the preliminarily modified multi-walled carbon nano-tube into a thionyl chloride solvent according to the mass ratio of 1:200, dropwise adding 5 drops of N, N-dimethylformamide as a catalyst, carrying out ultrasonic treatment for 0.5 hour under the power of 500W, and then refluxing for 12 hours at the temperature of 75 ℃ to obtain the modified multi-walled carbon nano-tube.
And pouring 42 parts of granulated blast furnace slag, 20 parts of calcined kaolin and 38 parts of quartz sand which are weighed into a stirrer, stirring for 120s to obtain a mixture, then placing 0.05 part of dispersing agent, 0.06 part of defoaming agent, 0.07 part of modified multi-walled carbon nanotube and 9 parts of water into 10 parts of composite alkali excitation solution, stirring for 120s, placing the mixture into 800W of power, performing ultrasonic treatment for 0.5 hour to obtain uniform mixed solution, then adding the uniform mixed solution into the mixture, stirring for 100s, finally adding 3 parts of silane coupling agent, stirring for 100s, then pouring, vibrating, and curing for 28d under the normal-temperature curing condition to obtain the high-impermeability geopolymer.
Example 3
The composite alkali activator in example 2 was used as the composite alkali activator, the calcined kaolin in example 2 was used as the calcined kaolin, and the modified multi-walled carbon nanotube in example 2 was used as the modified multi-walled carbon nanotube.
The preparation method comprises the steps of pouring 39 parts of weighed granulated blast furnace slag, 20 parts of calcined kaolin and 35 parts of quartz sand into a stirrer, stirring for 120s to obtain a mixture, then placing 0.05 part of a dispersing agent, 0.08 part of a defoaming agent, 0.07 part of a modified multi-walled carbon nanotube and 9 parts of water into 12 parts of a composite alkali excitation solution, stirring for 120s, placing the mixture into 700W power, performing ultrasonic treatment for 0.5 hour to obtain a uniform mixed solution, then adding the uniform mixed solution into the mixture, stirring for 120s, finally adding 2 parts of a silane coupling agent, stirring for 120s, then pouring, vibrating, and curing for 28d under the normal-temperature curing condition to obtain the high-impermeability geopolymer.
Example 4
The composite alkali activator in example 1 was used as the composite alkali activator, the calcined kaolin in example 1 was used as the calcined kaolin, and the modified multi-walled carbon nanotube in example 1 was used as the modified multi-walled carbon nanotube.
The preparation method comprises the steps of pouring 44 parts of granulated blast furnace slag, 15 parts of calcined kaolin and 35 parts of quartz sand which are weighed into a stirrer, stirring for 120s to obtain a mixture, then placing 0.05 part of a dispersing agent, 0.07 part of a defoaming agent, 0.08 part of a modified multi-walled carbon nanotube and 9 parts of water into 10 parts of a composite alkali excitation solution, stirring for 120s, placing the mixture into 800W power for ultrasonic treatment for 0.5 hour to obtain a uniform mixed solution, then adding the uniform mixed solution into the mixture, stirring for 100s, finally adding 3 parts of a silane coupling agent, stirring for 120s, then pouring, vibrating, and curing for 28d under the normal-temperature curing condition to obtain the high-impermeability geopolymer.
Example 5
The composite alkali activator in example 2 was used as the composite alkali activator, the calcined kaolin in example 2 was used as the calcined kaolin, and the modified multi-walled carbon nanotube in example 2 was used as the modified multi-walled carbon nanotube.
Pouring 40 parts of granulated blast furnace slag, 15 parts of calcined kaolin and 35 parts of quartz sand which are weighed into a stirrer, stirring for 120s to obtain a mixture, then placing 0.06 part of dispersing agent, 0.06 part of defoaming agent, 0.05 part of modified multi-walled carbon nano tube and 9 parts of water into 10 parts of composite alkali excitation solution, stirring for 120s, placing the mixture into 600W power, carrying out ultrasonic treatment for 0.5 hour to obtain uniform mixed solution, then adding the uniform mixed solution into the mixture, stirring for 100s, finally adding 12 parts of silane coupling agent, stirring for 100s, then pouring, vibrating, and curing for 28d under the normal-temperature curing condition to obtain the high-impermeability geopolymer.
The materials described in the above examples were tested according to the national standards "JC/T984-.
TABLE 1 test results for high barrier polymers
While embodiments of the present invention have been described above, the above description is intended to be exemplary, not exhaustive, and not limited to any embodiments carelessly. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (8)
1. The polymer with high impermeability is characterized by comprising the following components in parts by weight:
37-44 parts of granulated blast furnace slag, 10-20 parts of calcined kaolin, 33-40 parts of quartz sand, 10-12 parts of a composite alkali activator, 9-12 parts of water, 0.05-0.06 part of a dispersing agent, 0.06-0.08 part of a defoaming agent, 1-3 parts of a silane coupling agent and 0.06-0.08 part of a modified multi-walled carbon nanotube.
2. The polymer having high impermeability according to claim 1, wherein the granulated blast furnace slag contains 30 to 50 wt% of CaO and SiO2The content is 30-40 wt%, and the particle size is 2000-3000 meshes.
3. The polymer of claim 1, wherein the calcined kaolin is prepared by:
calcining kaolinite at 900 deg.C for 5-6 hr, and grindingGrinding, sieving to obtain powder with particle size of less than 200nm and Al content2O330-45 wt% of SiO2Is 30-35 wt%.
4. The polymer of claim 1, wherein the silica sand has a particle size of 40-80 mesh.
5. The polymer with high impermeability of claim 1, wherein the complex alkali activator is prepared by the following steps:
preparing water glass solution with initial modulus of 3.2-3.4 and solid content of 26-32%, adding solid sodium hydroxide of different quality to obtain sodium water glass with modulus of 1.6-1.8, and aging for 6-11 h.
6. The polymer of claim 1, wherein the silane coupling agent is any one or a mixture of KH550, KH560, KH 570.
7. The polymer of claim 1, wherein the modified multi-walled carbon nanotubes are prepared by:
placing the multi-walled carbon nano-tube in a mixed solution of concentrated nitric acid and concentrated sulfuric acid, and fully stirring; wherein the mass ratio of the multi-wall carbon nano-tube to the mixed solution is 1/100-1/200, and the volume ratio of the concentrated nitric acid to the concentrated sulfuric acid is 1/2-1/4;
standing after ultrasonic oscillation for 3-6 hours at 40-60 ℃, then diluting with deionized water, and performing centrifugal separation to obtain a precipitate; repeating the dilution, separation and precipitation until the pH of the resulting solution is greater than 7;
drying the obtained solution at 60-70 ℃ in a vacuum environment of 20-30Pa to obtain a preliminarily modified multi-walled carbon nanotube;
adding the preliminarily modified multi-walled carbon nano-tube into a thionyl chloride solvent according to the mass ratio of 1:200, dropwise adding 5 drops of N, N-dimethylformamide as a catalyst, carrying out ultrasonic treatment for 0.5-0.7 h under the power of 300-500W, and then refluxing for 12-20 h under the condition of 60-75 ℃ to obtain the modified multi-walled carbon nano-tube.
8. A method for preparing a polymer with high impermeability as claimed in any one of claims 1 to 7, characterized in that it comprises the following steps:
placing the defoaming agent, the dispersing agent, the multi-walled carbon nano tube and the water in the composite alkali-activated solution, stirring for 120-800 s, and then placing under the power of 600-800W for ultrasonic treatment for 0.8-0.9h to obtain a uniform mixed solution;
putting the granulated blast furnace slag, the calcined kaolin and the quartz sand into a stirring pot, and stirring for 60-100s to obtain a mixture;
adding the obtained mixed solution into the obtained mixture, stirring for 90-120s to obtain geopolymer slurry, adding a silane coupling agent, stirring for 90-120s, pouring, vibrating, and curing under standard curing conditions for 28 days to obtain the geopolymer with high impermeability.
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