CN115572087A - Geopolymer alkali activator and preparation method and application thereof - Google Patents
Geopolymer alkali activator and preparation method and application thereof Download PDFInfo
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- CN115572087A CN115572087A CN202211208794.1A CN202211208794A CN115572087A CN 115572087 A CN115572087 A CN 115572087A CN 202211208794 A CN202211208794 A CN 202211208794A CN 115572087 A CN115572087 A CN 115572087A
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- geopolymer
- alkali
- alkali activator
- surfactant
- activator
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- 229920000876 geopolymer Polymers 0.000 title claims abstract description 149
- 239000003513 alkali Substances 0.000 title claims abstract description 119
- 239000012190 activator Substances 0.000 title claims abstract description 114
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 63
- 239000002893 slag Substances 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 35
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 34
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004094 surface-active agent Substances 0.000 claims abstract description 33
- 239000003112 inhibitor Substances 0.000 claims abstract description 32
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 21
- 239000012670 alkaline solution Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 51
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical group CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 45
- 239000011521 glass Substances 0.000 claims description 29
- 239000011259 mixed solution Substances 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 22
- 239000002243 precursor Substances 0.000 claims description 14
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical group CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 claims description 10
- 238000001704 evaporation Methods 0.000 claims description 8
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000002585 base Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- XUJLWPFSUCHPQL-UHFFFAOYSA-N 11-methyldodecan-1-ol Chemical compound CC(C)CCCCCCCCCCO XUJLWPFSUCHPQL-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 8
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 235000019353 potassium silicate Nutrition 0.000 abstract description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000002910 solid waste Substances 0.000 abstract 1
- 239000002699 waste material Substances 0.000 description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 12
- 239000006004 Quartz sand Substances 0.000 description 11
- 239000010881 fly ash Substances 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 5
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 238000003760 magnetic stirring Methods 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 238000011161 development Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000011398 Portland cement Substances 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000002956 ash Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000004056 waste incineration Methods 0.000 description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical group [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229940045803 cuprous chloride Drugs 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
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
- 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
- C04B12/00—Cements not provided for in groups C04B7/00 - C04B11/00
- C04B12/005—Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
-
- 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
Abstract
The invention relates to the technical field of concrete engineering, in particular to a geopolymer alkali activator and a preparation method and application thereof, wherein the geopolymer alkali activator comprises the following raw materials: silicate raw materials, polymerization inhibitor, surfactant and strong alkaline solution; wherein the feeding concentration of the silicate is 30-50g/L; the feeding concentration of the polymerization inhibitor is 10-30mL/L; the feeding concentration of the surfactant is 5-10mg/L; the molar concentration of the strong alkali solution is 2-4 mol/L. The invention is prepared by adding silicate raw material, polymerization inhibitor and surfactant into strong alkaline solution and carrying out hydrothermal reaction. In the content range of the silicate raw material, the polymerization inhibitor, the surfactant and the alkaline solution, the modulus and the concentration of the obtained geopolymer excitant are high in controllability, and the slag content is low; compared with the traditional activator consisting of water glass and sodium hydroxide, the alkali activator takes silicate solid waste as a raw material, has a simple preparation process, and has the advantages of low energy consumption, low carbon emission and low cost.
Description
Technical Field
The invention relates to the technical field of concrete engineering, in particular to a geopolymer alkali activator and a preparation method and application thereof.
Background
Geopolymers, abbreviated as geopolymers, have the advantages of high strength, corrosion resistance, high temperature resistance, low carbon and environmental protection, and are widely considered as one of the best substitutes for the traditional portland cement.
However, geopolymer materials require the addition of an alkali activator to set and cure compared to conventional portland cement-based materials. And the use of alkali activators leads to an increase in the cost of geopolymer materials.
In addition, the excitant in the prior art is mainly a liquid alkali excitant which is formed by mixing water glass and sodium hydroxide. The water glass is often obtained by melting quartz sand at high temperature, which causes the problems of high energy consumption, high carbon emission and the like in the production of alkali activators.
Therefore, the alkali activator with low development cost, low energy consumption and low carbon emission has great significance.
Disclosure of Invention
Aiming at the technical problems, the invention provides a geopolymer alkali activator and a preparation method and application thereof. According to the invention, silicate is used as a raw material, and the alkaline activator is prepared by an alkaline hydrothermal method, so that the geopolymer alkaline activator has the advantages of low energy consumption and low carbon emission, and the problems of high energy consumption and high carbon emission of the alkaline activator are solved.
The invention adopts the following technical scheme:
in a first aspect, the invention provides a geopolymer alkali activator, which is prepared from the following raw materials: silicate raw materials, polymerization inhibitor, surfactant and strong alkaline solution; wherein the feeding concentration of the silicate raw material is 30-50g/L; the feeding concentration of the polymerization inhibitor is 10-30mL/L; the feeding concentration of the surfactant is 5-10mg/L; the molar concentration of the strong alkali solution is 2-4 mol/L. The above feed concentrations are all expressed relative to the concentration of the strong base solution.
Compared with the alkali activator in the prior art, the alkali activator can be prepared by carrying out mild hydrothermal reaction on the silicate raw material, the polymerization inhibitor, the surfactant and the alkaline solution with the concentration, and has the advantages of simple preparation process, low energy consumption, low carbon emission and modulus (SiO) 2 /Na 2 O) and strong concentration controllability, and the like, and has important meaning for customizing and flexibly adjusting excitant productsAnd (5) defining.
The geopolymer alkali activator can be prepared into a sodium alkali activator or a potassium alkali activator by adjusting a strong alkali solution to be sodium hydroxide or strong potassium oxide; the modulus of the geopolymer excitant product can be controlled to be in a suitable modulus range of 0.4-0.8 by adjusting the mass concentration of the silicate raw material added initially (the modulus of the traditional excitant is generally 0.6-1.2); the alkali concentration can be controlled by controlling the initial concentration of the alkali solution.
The geopolymer material prepared by the geopolymer alkali activator has the characteristic of high compressive strength, and also has excellent slurry easy-mixing characteristic (small viscosity), crack resistance and durability.
Preferably, the silicate raw material comprises glass slag, such as waste glass slag from waste incineration ash, glass fragments generated in the glass production and processing process, or common daily waste glass, so that the resource utilization of the waste silicate raw material is realized, and the purpose of environmental protection is achieved.
Preferably, the granularity of the glass slag is less than or equal to 48 mu m.
In the embodiment of the invention, the particle size of the glass slag is controlled to be below 48 mu m, so that the silicate raw material is easy to disperse, and the powdery and fine geopolymer alkali activator is obtained. The particle size requirement can be met by grinding with a grinder into a powder.
Because the components of the glass are relatively stable, and the geopolymer alkali-activator can be prepared from the glass slag from different sources according to the mass ratio of the components in the invention, the content of silicate in the glass slag is not limited at all.
Preferably, the polymerization inhibitor is triethylamine (C) 6 H 15 N)。
Triethylamine can rapidly react with free radicals to stop the reaction of a polymer chain, thereby preventing the self-polymerization of polymer monomers, reducing the generation of impurities and playing a key role in preparing a high-concentration alkali activator. Analytically pure triethylamine with purity of more than 99 percent is selected, so that the introduction of impurities can be avoided.
Preferably, the surfactant is nonylphenol or isomeric tridecanol polyoxyethylene ether.
In the embodiment of the invention, nonyl phenol or isotridecyl alcohol polyoxyethylene ether is used as a surfactant, so that a silicate raw material can be in full contact with a polymerization inhibitor and an alkaline solution to be fully reacted, and a geopolymer alkali activator is formed.
Preferably, the strong alkaline solution is a sodium hydroxide solution or a potassium hydroxide solution.
In the embodiment of the invention, the sodium type alkali activator can be obtained by adjusting the strong alkali solution to be sodium hydroxide; or regulating the strong alkali solution to be potassium hydroxide to obtain the potassium alkali excitant.
In a second aspect, the present invention also provides a preparation method of the geopolymer alkali activator, which at least comprises the following steps:
adding the silicate raw material, the polymerization inhibitor and the surfactant into the strong alkali solution, and mixing and stirring to obtain a precursor mixed solution;
and carrying out hydrothermal reaction on the precursor mixed solution in a sealed state to obtain the geopolymer alkali activator.
In the embodiment of the invention, silicate is used as a raw material, the geopolymer alkali activator is prepared by an alkaline hydrothermal method, and the hydrothermal reaction extract has high transparency and is substantially free of insoluble slag without filtration and impurity removal; the hydrothermal reaction condition is mild, the reaction time is short, and the energy consumption is saved; the closed environment can prevent the outside air from entering and avoid the introduction of impurities.
Preferably, the preparation method of the geopolymer alkali activator further comprises the following steps: evaporating the geopolymer alkali activator under the protection of inert gas until the weight is reduced by 1/4-1/3.
In the embodiment of the invention, under the protection of inert gas, the strong base excitant and CO in the air can be avoided 2 Reacting and carbonizing; the evaporation to 1/4-1/3 of the weight can reduce the water content in the product, so that the obtained concentrated geopolymer alkali-activator has better application effect. The inert gas may be selected to be nitrogen.
The embodiment of the invention provides a novel method for preparing a geopolymer alkali activator by an alkaline hydrothermal method.
Preferably, the conditions of the hydrothermal reaction include: the temperature is 140-200 ℃, the reaction time is 2-6 hours, and the pressure is 0.2-0.4MPa.
In the embodiment of the invention, the hydrothermal reaction condition is an optimal condition range obtained by experiment exploration, and under the condition, the prepared geopolymer exciting agent has the highest concentration and the optimal alkali excitation effect (the corresponding alkali-excited cementing material has the optimal performance, and the waste residue (byproduct) is the least).
Preferably, the strong alkali solution is sodium hydroxide to obtain a sodium type alkali activator; or
The alkali solution is potassium hydroxide to obtain the potassium alkali excitant.
The sodium alkali activator and the potassium alkali activator have similar effects, and can provide different product types for the geopolymer alkali activator.
Preferably, the surfactant is added to the strong alkali solution after being prepared into 1-10ml/L aqueous solution.
In a third aspect, the invention provides an application of the geopolymer alkali-activator or the geopolymer alkali-activator obtained by the preparation method in preparation of geopolymer materials.
In the embodiment of the invention, the geopolymer material prepared from the geopolymer alkali-activator, slag, fly ash and quartz stone has excellent compressive strength, and also has excellent slurry easy-mixing property (small viscosity), crack resistance and durability.
Drawings
FIG. 1 is an appearance diagram of a geopolymer alkali activator prepared in example 3 of the present invention.
FIG. 2 is a graph comparing the development of compressive strength of geopolymer alkali-activator prepared in example 3 of the present invention and geopolymer material prepared by conventional alkali-activator.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The invention provides a geopolymer alkali activator and a geopolymer material prepared from the geopolymer alkali activator. The geopolymer alkali activator comprises: adding waste glass slag serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and nonylphenol serving as a surfactant into the sodium hydroxide strong alkali solution; wherein, the waste glass slag is used after being ground and sieved by a 300-mesh sieve (the granularity is less than or equal to 48 mu m), and the feeding concentration is 30g/L; the feeding concentration of the polymerization inhibitor is 10mL/L; the feeding concentration of the surfactant is 5mg/L; the concentration of the sodium hydroxide solution was 2mol/L. The above feed concentrations were calculated relative to the sodium hydroxide solution.
The preparation method of the geopolymer alkali activator comprises the following steps:
adding glass slag serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and nonyl phenol serving as a surfactant into a sodium hydroxide strong alkali solution to obtain a precursor mixed solution;
transferring the precursor mixed solution into a magnetic stirring reaction kettle, carrying out hydrothermal reaction in a sealed state, and obtaining a mixed solution after the reaction time is 2 hours at the temperature of 140 ℃, the pressure of 0.2 MPa;
and transferring the mixed solution to a rotary evaporator, and evaporating under the protection of nitrogen gas flow until the weight is reduced by 1/4 to obtain the geopolymer alkali activator.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Example 2
The invention provides a geopolymer alkali activator and a geopolymer material prepared from the geopolymer alkali activator. The geopolymer alkali activator comprises: adding glass slag serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and nonylphenol serving as a surfactant into a sodium hydroxide strong alkali solution; wherein, the waste glass slag is used after being ground and sieved by a 300-mesh sieve (the granularity is less than or equal to 48 mu m), and the feeding concentration is 35g/L; the feeding concentration of the polymerization inhibitor is 15mL/L; the feeding concentration of the surfactant is 7mg/L; the concentration of the sodium hydroxide solution was 3mol/L. The above charge concentrations were calculated relative to the sodium hydroxide solution.
The preparation method of the geopolymer alkali activator comprises the following steps:
adding waste glass slag serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and nonylphenol serving as a surfactant into a sodium hydroxide strong alkali solution to obtain a precursor mixed solution;
transferring the precursor mixed solution into a magnetic stirring reaction kettle, carrying out hydrothermal reaction in a sealed state, and obtaining a mixed solution after the reaction time is 4 hours at the temperature of 160 ℃, the pressure of 0.3 MPa;
and transferring the mixed solution to a rotary evaporator, and evaporating under the protection of nitrogen gas flow until the weight is reduced by 7/25 to obtain the geopolymer alkali activator.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Example 3
The invention provides a geopolymer alkali activator and a geopolymer material prepared from the geopolymer alkali activator. The geopolymer alkali activator comprises: the waste glass slag separated from the waste incineration ash is silicate raw material, triethylamine is polymerization inhibitor, nonyl phenol is surfactant and sodium hydroxide is strong alkali solution; wherein, the waste glass slag is used after being ground and sieved by a 300-mesh sieve (the granularity is less than or equal to 48 mu m), and the feeding concentration is 40g/L; the feeding concentration of the polymerization inhibitor is 20mL/L; the feeding concentration of the surfactant is 9mg/L; the concentration of the sodium hydroxide solution was 4mol/L. The above feed concentrations were calculated relative to the sodium hydroxide solution.
The preparation method of the geopolymer alkali activator comprises the following steps:
adding waste glass slag serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and nonyl phenol serving as a surfactant into a sodium hydroxide strong alkali solution, and mixing and stirring to obtain a precursor mixed solution;
transferring the precursor mixed solution into a magnetic stirring reaction kettle, carrying out hydrothermal reaction in a sealed state, and obtaining a mixed solution after 5 hours of reaction at the temperature of 180 ℃, the pressure of 0.35 MPa;
and transferring the mixed solution to a rotary evaporator, and evaporating under the protection of nitrogen gas flow until the weight is reduced by 3/10 to obtain the geopolymer alkali activator.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Example 4
The invention provides a geopolymer alkali activator and a geopolymer material prepared from the geopolymer alkali activator. The geopolymer alkali activator comprises: ordinary daily waste glass is used as a silicate raw material, triethylamine is used as a polymerization inhibitor, isomeric tridecanol polyoxyethylene ether is used as a surfactant and a potassium hydroxide strong base solution; wherein, the waste glass slag is used after being ground and sieved by a 300-mesh sieve (the granularity is less than or equal to 48 mu m), and the feeding concentration is 45g/L; the feeding concentration of the polymerization inhibitor is 25mL/L; the feeding concentration of the surfactant is 9.5mg/L; the concentration of the potassium hydroxide solution was 3mol/L.
The preparation method of the geopolymer alkali activator comprises the following steps:
adding ordinary daily waste glass serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and isomeric tridecanol polyoxyethylene ether serving as a surfactant into a potassium hydroxide strong alkali solution, and mixing and stirring to obtain a precursor mixed solution;
transferring the precursor mixed solution into a magnetic stirring reaction kettle, carrying out hydrothermal reaction in a sealed state, and obtaining a mixed solution after the reaction time is 5.5 hours at the temperature of 190 ℃, the pressure of 0.38 MPa;
and transferring the mixed solution to a rotary evaporator, and evaporating under the protection of nitrogen gas flow until the weight is reduced by 31/100 to obtain the geopolymer alkali activator.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Example 5
The invention provides a geopolymer alkali activator and a geopolymer material prepared from the geopolymer alkali activator. The geopolymer alkali activator. The geopolymer alkali activator comprises: ordinary daily waste glass is used as a silicate raw material, triethylamine is used as a polymerization inhibitor, isomeric tridecanol polyoxyethylene ether is used as a surfactant and a potassium hydroxide strong base solution; wherein, the waste glass slag is used after being ground and sieved by a 300-mesh sieve (the granularity is less than or equal to 48 mu m), and the feeding concentration is 50g/L; the feeding concentration of the polymerization inhibitor is 30mL/L; the feeding concentration of the surfactant is 10mg/L; the concentration of the potassium hydroxide solution was 3mol/L. The above feed concentrations were calculated relative to the sodium hydroxide solution.
The preparation method of the geopolymer alkali activator comprises the following steps:
adding ordinary daily waste glass serving as a silicate raw material, triethylamine serving as a polymerization inhibitor and isomeric tridecanol polyoxyethylene ether serving as a surfactant into a potassium hydroxide strong alkali solution, and mixing and stirring to obtain a precursor mixed solution;
transferring the precursor mixed solution into a magnetic stirring reaction kettle, carrying out hydrothermal reaction in a sealed state, and obtaining a mixed solution after 6 hours of reaction at the temperature of 200 ℃, the pressure of 0.4 MPa;
and transferring the mixed solution to a rotary evaporator, and evaporating under the protection of nitrogen gas flow until the weight is reduced by 1/3 to obtain the geopolymer alkali activator.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Comparative example 1
The prior art conventional excitant and geopolymer material prepared by the conventional excitant. The traditional excitant is prepared by mixing 40 percent of 8mol/L sodium hydroxide solution and 60 percent of 51-degree (Baume degree) water glass.
Preparation of geopolymer material:
60 parts of the conventional excitant prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Comparative example 2
The polymerization inhibitor of the geopolymer alkali activator in example 3 was replaced with cuprous chloride, and the rest of the composition was the same as in example 3.
The preparation method of the geopolymer alkali activator is the same as that of the example 3.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Comparative example 3
The surfactant of the geopolymer alkali activator in example 3 was replaced with sodium dodecylbenzenesulfonate, and the rest of the components were the same as in example 3.
The preparation method of the geopolymer alkali activator is the same as that of the example 3.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Comparative example 4
The geopolymer alkali activator is the same as in example 3.
The conditions of hydrothermal reaction of the geopolymer alkali activator in the embodiment 3 are changed as follows: the reaction time was 2 hours at a temperature of 120 ℃ and a pressure of 0.15MPa, and the same procedure as in example 3 was repeated to obtain a geopolymer alkali activator.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Comparative example 5
The geopolymer alkali activator is the same as in example 3.
The conditions of hydrothermal reaction of the geopolymer alkali activator in example 3 were changed as follows: the reaction time was 6.5 hours at a temperature of 300 ℃ and a pressure of 0.5MPa, and the geopolymer alkali activator was obtained in the same manner as in example 3.
Preparation of geopolymer material:
60 parts of geopolymer alkali activator prepared above, 50 parts of slag, 50 parts of fly ash and 200 parts of quartz sand are used to prepare the geopolymer material.
Verification example 1
The appearance of the geopolymer alkali activator prepared in example 3 was observed, and the results are shown in FIG. 1.
FIG. 1 is an appearance diagram of a geopolymer alkali activator prepared in example 3 of the present invention.
As can be seen from FIG. 1, the geopolymer alkali activator prepared in example 3 of the present invention has high transparency of appearance, substantially no insoluble residue, and no need of filtration to remove impurities.
The compression strength development of the geopolymer alkali-activator prepared in example 3 is compared with that of the geopolymer material prepared by the traditional alkali-activator, and the result is shown in FIG. 2.
FIG. 2 is a graph comparing the development of compressive strength of geopolymer alkali-activator prepared in example 3 of the present invention and geopolymer material prepared by conventional alkali-activator.
As can be seen from FIG. 2, the compression strength of the geopolymer material prepared by the geopolymer alkali-activator in example 3 of the present invention is about 48MPa in 28d, and the compression strength of the geopolymer material prepared by the comparative example 1 is about 47.8MPa in 28d, it can be seen that the compression strength of the geopolymer material prepared by the geopolymer alkali-activator prepared by the present invention is obviously stronger than that of the geopolymer material prepared by the alkali-activator in the prior art.
Verification example 2
The geopolymer materials prepared in examples 1-5 and the geopolymer materials prepared in comparative examples 1-5 are subjected to pressure intensity test, and are tested and tested by the GB/T17671-1999 cement mortar strength test method (ISO method), and the performance indexes are shown in Table 1.
TABLE 1 Performance index
In Table 1, the slag yield means: mass percent relative to the input amount of the silicate raw material.
As can be seen from Table 1, the compression strength of the geopolymer material prepared by the geopolymer excitant obtained by the invention is obviously better than that of the geopolymer materials prepared by the comparative examples 1-5.
As can be further seen from Table 2, the viscosity, crack resistance and durability of the geopolymer alkali activator prepared in example 3 of the invention and the geopolymer material prepared by the traditional alkali activator are obviously better than those of comparative examples 1-5.
In comparison with the geopolymer materials of examples 1 to 5, the polymerization inhibitor of the present invention was replaced with other substances, and the polymerization inhibiting effect of the triethylamine of the present invention, which is preferred, was not achieved.
Comparative example 3 in comparison with the geopolymer materials of examples 1-5, replacement of the polymerization inhibitor of the present invention with other surfactants also failed to achieve the technical effect of the nonylphenol or isotridecanol polyoxyethylene ether of the present invention as a surfactant.
Comparative examples 4 to 5 in comparison with the geopolymer materials of examples 1 to 5, the slag yields of comparative examples 4 and 5 were 46.9% and 23.7%, and the slag yields of examples 1 to 5 were 5.7%, 5.2%, 6.8%, 11.3%, and 14.8%, respectively, and it was found that if the hydrothermal reaction conditions of the present invention were changed so as not to fall within the hydrothermal reaction conditions of the present invention, the slag yield of the geopolymer material was significantly increased, the compressive strength of the geopolymer activator 28d thus obtained was reduced, and the strength of the resulting cement was significantly reduced.
In conclusion, the geopolymer excitant obtained by the invention has the advantages of strong modulus and concentration controllability, low energy consumption and low carbon emission.
The geopolymer material prepared by the geopolymer excitant has excellent compressive strength, and also has excellent slurry easy-mixing characteristic (small viscosity), crack resistance and durability. The method can be used as the best substitute of the traditional portland cement, realizes low-carbon emission, takes the waste glass slag as a silicate raw material, has low cost, and realizes the resource utilization of the waste glass slag to achieve the aim of environmental protection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The geopolymer alkali activator is characterized in that the preparation raw materials comprise the following components: silicate raw materials, polymerization inhibitor, surfactant and strong alkaline solution; wherein the feeding concentration of the silicate raw material is 30-50g/L; the feeding concentration of the polymerization inhibitor is 10-30mL/L; the feeding concentration of the surfactant is 5-10mg/L; the molar concentration of the strong alkali solution is 2-4 mol/L.
2. The geopolymer alkali activator according to claim 1, wherein the silicate raw material comprises glass slag.
3. The geopolymer alkali activator according to claim 2, wherein the grain size of the glass slag is less than or equal to 48 μm.
4. The geopolymer base activator according to claim 1, wherein the polymerization inhibitor is triethylamine.
5. The geopolymer alkali activator according to claim 1, wherein the surfactant is nonylphenol or isotridecanol polyoxyethylene ether.
6. The geopolymer alkali activator according to claim 1, wherein the strong alkali solution is a sodium hydroxide solution or a potassium hydroxide solution.
7. The method for producing the geopolymer alkali-activator according to any one of claims 1 to 6, characterized by comprising at least the steps of:
adding the silicate raw material, the polymerization inhibitor and the surfactant into the strong alkali solution, and mixing and stirring to obtain a precursor mixed solution;
and carrying out hydrothermal reaction on the precursor mixed solution in a sealed state to obtain the geopolymer alkali activator.
8. The method for preparing the geopolymer alkali activator according to claim 7, further comprising: evaporating the geopolymer alkali activator under the protection of inert gas until the weight is reduced by 1/4-1/3.
9. The method for producing a geopolymer alkali activator according to claim 7,
the conditions of the hydrothermal reaction include: the temperature is 140-200 ℃, the reaction time is 2-6 hours, and the pressure is 0.2-0.4MPa.
10. Use of the geopolymer alkali activator according to any one of claims 1 to 6 or obtained by the preparation method according to any one of claims 7 to 9 in the preparation of geopolymer materials.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07133147A (en) * | 1991-12-25 | 1995-05-23 | Hera Corp:The | Geopolymer-modified gypsum base building material |
| CN110451865A (en) * | 2019-09-18 | 2019-11-15 | 安徽理工大学 | A kind of geo-polymer and heat preservation and soundproof damping plate based on printing and dyeing sludge preparation |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07133147A (en) * | 1991-12-25 | 1995-05-23 | Hera Corp:The | Geopolymer-modified gypsum base building material |
| CN110451865A (en) * | 2019-09-18 | 2019-11-15 | 安徽理工大学 | A kind of geo-polymer and heat preservation and soundproof damping plate based on printing and dyeing sludge preparation |
Non-Patent Citations (1)
| Title |
|---|
| 杨敬斌等: ""碱胶凝材料水化产物C- A- S- H与N- A- S- H的研究进展"" * |
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