CN110218035B - Preparation method of plastic deformation geopolymer material - Google Patents
Preparation method of plastic deformation geopolymer material Download PDFInfo
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- 229920000876 geopolymer Polymers 0.000 title claims abstract description 59
- 239000000463 material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000004033 plastic Substances 0.000 title claims description 14
- 229920003023 plastic Polymers 0.000 title claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 69
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 57
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 55
- 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 30
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000008235 industrial water Substances 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000007791 liquid phase Substances 0.000 claims description 34
- 239000007790 solid phase Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 24
- 239000002002 slurry Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 9
- 239000003153 chemical reaction reagent Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 4
- 235000012211 aluminium silicate Nutrition 0.000 claims description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims 6
- 239000006185 dispersion Substances 0.000 claims 2
- 230000008859 change Effects 0.000 abstract description 17
- 238000005338 heat storage Methods 0.000 abstract description 10
- 239000003513 alkali Substances 0.000 abstract description 4
- 239000002253 acid Substances 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000005266 casting Methods 0.000 abstract description 2
- 231100000956 nontoxicity Toxicity 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 27
- 239000012071 phase Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 9
- 239000000126 substance Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000007704 transition Effects 0.000 description 5
- 239000012782 phase change material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- 239000011232 storage material Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- CQBLUJRVOKGWCF-UHFFFAOYSA-N [O].[AlH3] Chemical compound [O].[AlH3] CQBLUJRVOKGWCF-UHFFFAOYSA-N 0.000 description 1
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical compound [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910001579 aluminosilicate mineral Inorganic materials 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 239000002969 artificial stone Substances 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 229920003041 geopolymer cement Polymers 0.000 description 1
- 159000000011 group IA salts Chemical class 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- 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
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Consolidation Of Soil By Introduction Of Solidifying Substances Into Soil (AREA)
- Soil Conditioners And Soil-Stabilizing Materials (AREA)
Abstract
本发明公开了一种可塑性变形地质聚合物材料的制备方法，该地质聚合物材料由偏高岭土、工业水玻璃、九水合硅酸钠、氢氧化钠按一定质量分数比混合浇注成型，常温养护而成。本发明制备工艺简单，制备得到的地质聚合物材料具有无毒、低成本、早强、快硬、耐酸耐碱、绿色环保、性能稳定的特点，可满足低温相变储热领域的地质聚合物材料，有望在相变储热领域得到应用。The invention discloses a preparation method of a plastically deformable geopolymer material. The geopolymer material is formed by mixing and casting metakaolin, industrial water glass, sodium silicate nonahydrate and sodium hydroxide according to a certain mass fraction ratio, and curing at room temperature to form it. to make. The preparation process of the invention is simple, the prepared geopolymer material has the characteristics of non-toxicity, low cost, early strength, fast hardening, acid and alkali resistance, environmental protection and stable performance, and can meet the geopolymer in the field of low temperature phase change heat storage. The material is expected to be applied in the field of phase change heat storage.
Description
技术领域technical field
本发明属于材料工程技术领域，涉及一种可塑性变形地质聚合物材料的制备方法。The invention belongs to the technical field of material engineering, and relates to a preparation method of a plastically deformable geopolymer material.
背景技术Background technique
地质聚合物(Geopolymer)是在强碱或强酸条件下，将含无定形SiO2和Al2O3的铝硅酸盐矿物与碱溶液、碱性盐溶液或磷酸、磷酸盐溶液混合，经过缩聚反应生成的由硅氧四面体、铝氧四面体或磷氧四面体构成的无定形三维网络凝胶体。地质聚合物材料的应用可追溯到古代，即以高岭土、白云岩或石灰岩与盐湖成分Na2CO3、草木灰成分K2CO3以及硅石的混合物，加水拌和后产生强碱NaOH和KOH，与其它组分发生反应，生成矿物聚合粘结剂而制成人造石。由于该材料体积密度小（1.3~1.9g·cm-3），轻质高强；耐腐蚀性、耐水热性、体积收缩小、高温热稳定性及耐久性良好；同时具有绿色环保等优点。使其逐渐成为近年来国际上研究非常活跃的材料之一。但其抗弯、抗拉强度低，抗冲击强度差，脆性大，易开裂等问题，这些都限制了其发展与应用。Geopolymer is a mixture of aluminosilicate minerals containing amorphous SiO 2 and Al 2 O 3 with alkaline solution, alkaline salt solution or phosphoric acid and phosphate solution under strong alkali or strong acid conditions, and then undergoes polycondensation. The amorphous three-dimensional network gel formed by the reaction is composed of silicon-oxygen tetrahedron, aluminum-oxygen tetrahedron or phosphorus-oxygen tetrahedron. The application of geopolymer materials can be traced back to ancient times, that is, the mixture of kaolin, dolomite or limestone with salt lake component Na 2 CO 3 , plant ash component K 2 CO 3 and silica, after mixing with water, produces strong alkali NaOH and KOH, and other The components react to form a mineral aggregated binder to make artificial stone. Due to its small bulk density (1.3~1.9g·cm -3 ), light weight and high strength, corrosion resistance, hydrothermal resistance, small volume shrinkage, good high temperature thermal stability and durability, it also has the advantages of green environmental protection. It has gradually become one of the most active materials in international research in recent years. However, its low bending and tensile strength, poor impact strength, high brittleness, and easy cracking limit its development and application.
相变材料是指随温度变化而改变形态并能提供潜热的物质。目前应用较多的是固-液相变材料，相变材料由固态变为液态或由液态变为固态的过程称为相变过程，这时相变材料将吸收或释放大量的潜热。国内外有研究表明，当地质聚合物制成泥膏状时具有良好的可塑性。有研究学者研究了地质聚合物混凝土的冲击变形特性，研究表明采用矿渣、粉煤灰等地质聚合物材料代替水泥作为胶凝材料，并以硅酸钠和氢氧化钠为激发剂，可以制备变形性能良好、能相变储热的地质聚合物材料。Phase change materials refer to substances that change shape with temperature changes and can provide latent heat. At present, solid-liquid phase change materials are widely used. The process of phase change materials from solid to liquid or from liquid to solid is called the phase change process. At this time, the phase change material will absorb or release a large amount of latent heat. Studies at home and abroad have shown that geopolymers have good plasticity when they are made into mud paste. Some researchers have studied the impact deformation characteristics of geopolymer concrete. The research shows that geopolymer materials such as slag and fly ash are used instead of cement as cementing materials, and sodium silicate and sodium hydroxide are used as activators to prepare deformation. Geopolymer material with good performance and phase change heat storage.
发明专利（专利号201711455186.X）公开了一种聚氯乙烯相变储热板材的制备方法，通过该法制备的相变储热材料储热能力有所提高，但聚氯乙烯在高温明火下分解产生有毒气体，在一些领域存在风险。专利号CN201810889301.2是一种有机/无机复合储能相变材料的制备方法，该制备方法具有一定的相变储热性能，但该法所制备的材料有腐蚀性、成本较高，这限制了其发展应用。The invention patent (Patent No. 201711455186.X) discloses a preparation method of a polyvinyl chloride phase change heat storage plate. The heat storage capacity of the phase change heat storage material prepared by this method has been improved, but the polyvinyl chloride is under high temperature and open fire. Decomposition produces toxic gases, which are a risk in some areas. Patent No. CN201810889301.2 is a preparation method of an organic/inorganic composite energy storage phase change material. The preparation method has a certain phase change heat storage performance, but the material prepared by this method is corrosive and has a high cost, which limits the its development application.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于针对现有相变储热材料存在的有腐蚀性、高温分解、成本高和不可塑变形等缺陷，提供一种可塑性变形地质聚合物材料的制备方法，本发明制备工艺简单，制备得到的地质聚合物材料具有无毒、低成本、早强、快硬、耐酸耐碱、绿色环保、性能稳定的特点，有望在相变储热领域得到应用。The purpose of the present invention is to provide a preparation method of plastically deformable geopolymer material in view of the defects of corrosiveness, high temperature decomposition, high cost and non-plastic deformation existing in the existing phase change heat storage materials, and the preparation process of the present invention is simple, The prepared geopolymer material has the characteristics of non-toxicity, low cost, early strength, fast hardening, acid and alkali resistance, environmental protection and stable performance, and is expected to be applied in the field of phase change heat storage.
本发明的方案是通过这样实现的：The solution of the present invention is achieved by:
一种可塑性变形地质聚合物材料的制备方法，主要由偏高岭土、工业水玻璃、九水合硅酸钠、氢氧化钠按一定质量比混合浇注成型，常温养护而成。A method for preparing a plastically deformable geopolymer material is mainly formed by mixing metakaolin, industrial water glass, sodium silicate nonahydrate, and sodium hydroxide according to a certain mass ratio, and curing at room temperature.
作为本发明的进一步说明，可塑性变形地质聚合物材料的制备方法具体包括以下步骤：As a further description of the present invention, the preparation method of the plastically deformable geopolymer material specifically includes the following steps:
（a）水玻璃溶液的制备：按照质量比约为（3.3~3.5）: 1称取工业水玻璃和氢氧化钠，将工业水玻璃和氢氧化钠进行超声搅拌溶解配成固定模数1.0的水玻璃溶液；(a) Preparation of water glass solution: According to the mass ratio of about (3.3~3.5): 1, weigh industrial water glass and sodium hydroxide, and ultrasonically stir and dissolve the industrial water glass and sodium hydroxide to prepare a fixed modulus of 1.0. water glass solution;
（b）液相L的制备：按照质量比约为（2.5～4.7）: 1称取水玻璃溶液与九水合硅酸钠，利用搅拌子将水玻璃溶液与九水合硅酸钠进行超声搅拌混合60min、静置一段时间后得到液相L；(b) Preparation of liquid phase L: According to the mass ratio of about (2.5～4.7): 1 Weigh the water glass solution and sodium silicate nonahydrate, and use a stirrer to ultrasonically stir and mix the water glass solution and sodium silicate nonahydrate for 60 minutes , to obtain liquid phase L after standing for a period of time;
（c）以偏高岭土为固相S，将固相S与液相L置于高速分散机中，在转速为2000r/min的转速条件下混合搅拌15min即可得到可塑性变形地质聚合物浆料，其中，液相L与固相S质量比例约为：L : S=2.95～325.52；(c) Using metakaolin as the solid phase S, placing the solid phase S and the liquid phase L in a high-speed disperser, and mixing and stirring for 15 minutes at a rotational speed of 2000 r/min to obtain a plastically deformable geopolymer slurry, Among them, the mass ratio of liquid phase L to solid phase S is about: L : S=2.95～325.52;
（d）将可塑性变形地质聚合物浆料浇注至模具，在常温条件下放置30min后脱模，然后进行养护即得到可塑性变形地质聚合物材料。(d) The plastically deformable geopolymer slurry is poured into the mold, placed at room temperature for 30 minutes, then demolded, and then cured to obtain the plastically deformable geopolymer material.
作为本发明的进一步说明，所述偏高岭土是将高岭土在800℃的条件下煅烧2h得到的粉体，煅烧得到的偏高岭土中各成分质量百分比含量为：SiO2：52.89%，Al2O3：43.50%，K2O：1.8%，Fe2O3：1.38%，MgO：0.43%；所述的九水合硅酸钠为固体颗粒且为含质量分数96%的实验室分析纯试剂，所述的氢氧化钠为含质量分数96%的实验室分析纯试剂。As a further description of the present invention, the metakaolin is a powder obtained by calcining kaolin at 800° C. for 2 hours, and the mass percentage content of each component in the calcined metakaolin is: SiO 2 : 52.89%, Al 2 O 3 : 43.50%, K 2 O: 1.8%, Fe 2 O 3 : 1.38%, MgO: 0.43%; the sodium silicate nonahydrate is a solid particle and is a laboratory analytical reagent with a mass fraction of 96%. The sodium hydroxide described is a laboratory analytical reagent with a mass fraction of 96%.
作为本发明的进一步说明，所述的模具规格为20×20×20mm。As a further description of the present invention, the size of the mold is 20×20×20mm.
作为本发明的进一步说明，所述的工业水玻璃模数为3.31。As a further description of the present invention, the modulus of the industrial water glass is 3.31.
本发明实现的技术原理是：The technical principle realized by the present invention is:
本发明中偏高岭土提供硅铝源，偏高岭土在水玻璃溶液的作用下硅氧键和铝氧键发生断裂-重组反应，再聚合生成地质聚合物。在本发明的原料中工业水玻璃主要成分是硅酸钠，其分子式为Na2SiO3。九水合硅酸钠分子式为Na2SiO3·9H2O，九水合硅酸钠是荷电载体，分子量小，通过电荷吸附、氢键及范德华力等作用吸附在物质颗粒的表面，使得颗粒表面产生化学吸附特性，有作为黏合剂和分散剂的作用；能够使得制备的地质聚合物各个组分之间相容，提高其稳定性，并且九水合硅酸钠熔点约为40-48℃而工业水玻璃的熔点约为1089℃，九水合硅酸钠在较低温度（如30~40℃时）下会释放结晶水变成液体或膏状，从而促进地质聚合物的状态随着温度的变化而变化。该地质聚合物材料在常温下可在短时间内凝结硬化，并且具有一定的抗压强度；再将此成型材料在高于室温的环境下（约60℃左右）放置一段时间后，该材料会变软并析出少量水分。此种可塑性变形地质聚合物材料根据温度的变化，可呈现不同的状态：在室温下处于具有固定形态的固体物质，而在高温下处于固液相共存似泥巴状态的物质，并且物质的两种状态可以根据外界环境温度的变换进行多次转化，从而具有可塑性变形。In the present invention, the metakaolin provides a silicon-alumina source, and the metakaolin undergoes a fracture-recombination reaction under the action of the water glass solution, and then polymerizes to form a geopolymer. In the raw material of the present invention, the main component of industrial water glass is sodium silicate, and its molecular formula is Na 2 SiO 3 . The molecular formula of sodium silicate nonahydrate is Na 2 SiO 3 9H 2 O. Sodium silicate nonahydrate is a charge carrier with small molecular weight. It produces chemical adsorption properties and acts as a binder and dispersant; it can make the various components of the prepared geopolymer compatible and improve its stability, and the melting point of sodium silicate nonahydrate is about 40-48 ° C and industrial The melting point of water glass is about 1089 ℃, and sodium silicate nonahydrate will release crystal water at lower temperature (such as 30~40 ℃) and become liquid or paste, thus promoting the state of geopolymer to change with temperature and change. The geopolymer material can be solidified and hardened in a short time at normal temperature, and has a certain compressive strength; after the molding material is placed in an environment higher than room temperature (about 60°C) for a period of time, the material will Softened and released a little moisture. This plastically deformable geopolymer material can show different states according to the change of temperature: it is a solid substance with a fixed form at room temperature, and at high temperature, it is a substance in a state of coexistence of solid and liquid phases like mud, and the two kinds of substances. The state can be transformed multiple times according to the change of the external ambient temperature, so that it has plastic deformation.
本发明具备以下良好效果：The present invention has the following good effects:
1.本发明采用常温浇注成型，常温养护，工艺简单，无毒无污染。1. The present invention adopts normal temperature casting molding, normal temperature maintenance, simple process, non-toxic and pollution-free.
2.本发明碱激发活性材料、偏高岭土、工业水玻璃等原材料来源广泛或为工业废渣，成本低，并且可解决废弃物利用问题。2. The raw materials such as the alkali-excited active material, metakaolin, industrial water glass, etc. of the present invention are widely sourced or are industrial waste residues, the cost is low, and the problem of waste utilization can be solved.
3.本发明中制备得到的可塑性变形地质聚合物材料当外界温度发生改变时，可塑性变形地质聚合物的形态就会发生改变，在相变储热领域有一定的应用前景。3. When the external temperature of the plastically deformable geopolymer material prepared in the present invention changes, the form of the plastically deformable geopolymer will change, which has certain application prospects in the field of phase change heat storage.
具体实施方式Detailed ways
以下结合实施例描述本发明一种可塑性变形地质聚合物材料的制备方法，这些描述并不是对本发明内容作进一步的限定。The following describes a method for preparing a plastically deformable geopolymer material of the present invention with reference to the examples, and these descriptions are not intended to further limit the content of the present invention.
（1）本发明中的偏高岭土是将高岭土在800℃的条件下煅烧2h得到的粉体，煅烧得到的偏高岭土的各化学成分质量百分比含量如下表。(1) The metakaolin in the present invention is a powder obtained by calcining kaolin at 800°C for 2 hours. The mass percentage content of each chemical component of the metakaolin obtained by calcining is as follows.
（2）本发明中，九水合硅酸钠为固体颗粒且为含质量分数96%的实验室分析纯试剂，氢氧化钠为含质量分数96%的实验室分析纯试剂。(2) In the present invention, sodium silicate nonahydrate is a solid particle and is a laboratory analytically pure reagent with a mass fraction of 96%, and sodium hydroxide is a laboratory analytically pure reagent with a mass fraction of 96%.
实施例1：Example 1:
（a）水玻璃溶液的制备：按照每100g的模数为3.31的工业水玻璃称取质量分数96%氢氧化钠28.85g，将称好的工业水玻璃和氢氧化钠进行超声搅拌溶解配成固定模数1.0的水玻璃溶液；(a) Preparation of water glass solution: Weigh 28.85 g of 96% sodium hydroxide by mass per 100 g of industrial water glass with a modulus of 3.31, and dissolve the weighed industrial water glass and sodium hydroxide by ultrasonic stirring to prepare A water glass solution with a fixed modulus of 1.0;
（b）液相L的制备：按照每133.58g的水玻璃溶液称取九水合硅酸钠27.40g，利用搅拌子将称好的水玻璃溶液与九水合硅酸钠进行超声搅拌混合60min、静置4小时后得到液相L；(b) Preparation of liquid phase L: Weigh 27.40 g of sodium silicate nonahydrate per 133.58 g of water glass solution, and use a stirrer to ultrasonically stir and mix the weighed water glass solution and sodium silicate nonahydrate for 60 min. After 4 hours, liquid phase L was obtained;
（c）以偏高岭土为固相S，称取160.98g液相L和32.48g偏高岭土固相S，将固相S与液相L置于高速分散机中，在转速为2000r/min的转速条件下混合搅拌15min即可得到可塑性变形地质聚合物浆料；(c) Using metakaolin as the solid phase S, weigh 160.98g liquid phase L and 32.48g metakaolin solid phase S, put the solid phase S and liquid phase L in a high-speed disperser, at a speed of 2000r/min The plastic deformation geopolymer slurry can be obtained by mixing and stirring for 15 minutes under the conditions;
（d）将可塑性变形地质聚合物浆料浇注至20×20×20mm模具，在常温条件下放置30min后脱模，然后进行养护即得到可塑性变形地质聚合物材料。(d) The plastically deformable geopolymer slurry was poured into a 20×20×20 mm mold, placed at room temperature for 30 minutes, and then demolded, and then cured to obtain a plastically deformable geopolymer material.
对常温养护后的可塑性变形地质聚合物材料进行测定，其抗压强度达到19.75Mpa，DSC测试结果表明，所制备的可塑性变形地质聚合物材料的相变温度为60℃。The compressive strength of the plastically deformable geopolymer material after normal temperature curing was measured, and its compressive strength reached 19.75Mpa. The DSC test results showed that the phase transition temperature of the prepared plastically deformable geopolymer material was 60℃.
实施例2：Example 2:
（a）水玻璃溶液的制备：按照每100g的模数为3.31的工业水玻璃称取质量分数96%氢氧化钠28.85g，将称好的工业水玻璃和氢氧化钠进行超声搅拌溶解配成固定模数1.0的水玻璃溶液；(a) Preparation of water glass solution: Weigh 28.85 g of 96% sodium hydroxide by mass per 100 g of industrial water glass with a modulus of 3.31, and dissolve the weighed industrial water glass and sodium hydroxide by ultrasonic stirring to prepare A water glass solution with a fixed modulus of 1.0;
（b）液相L的制备：按照每128.85g的水玻璃溶液称取九水合硅酸钠37.40g，利用搅拌子将称好的水玻璃溶液与九水合硅酸钠进行超声搅拌混合60min、静置4小时后得到液相L；(b) Preparation of liquid phase L: Weigh 37.40 g of sodium silicate nonahydrate per 128.85 g of water glass solution, and use a stirrer to ultrasonically stir and mix the weighed water glass solution and sodium silicate nonahydrate for 60 min. After 4 hours, liquid phase L was obtained;
（c）以偏高岭土为固相S，称取166.25g液相L和32.48g偏高岭土固相S，将固相S与液相L置于高速分散机中，在转速为2000r/min的转速条件下混合搅拌15min即可得到可塑性变形地质聚合物浆料；(c) Take metakaolin as solid phase S, weigh 166.25g liquid phase L and 32.48g metakaolin solid phase S, place solid phase S and liquid phase L in a high-speed disperser, and rotate at a speed of 2000r/min The plastic deformation geopolymer slurry can be obtained by mixing and stirring for 15 minutes under the conditions;
（d）将可塑性变形地质聚合物浆料浇注至20×20×20mm模具，在常温条件下放置30min后脱模，然后进行养护即得到可塑性变形地质聚合物材料。(d) The plastically deformable geopolymer slurry was poured into a 20×20×20 mm mold, placed at room temperature for 30 minutes, and then demolded, and then cured to obtain a plastically deformable geopolymer material.
对常温养护后的可塑性变形地质聚合物材料进行测定，其抗压强度达到22.74Mpa，DSC测试结果表明，所制备的可塑性变形地质聚合物材料的相变温度为66℃。The compressive strength of the plastically deformable geopolymer material after normal temperature curing was measured, and its compressive strength reached 22.74Mpa. The DSC test results showed that the phase transition temperature of the prepared plastically deformable geopolymer material was 66℃.
实施例3：Example 3:
（a）水玻璃溶液的制备：按照每100g的模数为3.31的工业水玻璃称取质量分数96%氢氧化钠28.85g，将称好的工业水玻璃和氢氧化钠进行超声搅拌溶解配成固定模数1.0的水玻璃溶液；(a) Preparation of water glass solution: Weigh 28.85 g of 96% sodium hydroxide by mass per 100 g of industrial water glass with a modulus of 3.31, and dissolve the weighed industrial water glass and sodium hydroxide by ultrasonic stirring to prepare A water glass solution with a fixed modulus of 1.0;
（b）液相L的制备：按照每128.85g的水玻璃溶液称取九水合硅酸钠27.40g，利用搅拌子将称好的水玻璃溶液与九水合硅酸钠进行超声搅拌混合60min、静置4小时后得到液相L；(b) Preparation of liquid phase L: Weigh 27.40 g of sodium silicate nonahydrate per 128.85 g of water glass solution, and use a stirrer to ultrasonically stir and mix the weighed water glass solution and sodium silicate nonahydrate for 60 min. After 4 hours, liquid phase L was obtained;
（c）以偏高岭土为固相S，称取156.25g液相L和34.48g偏高岭土固相S，将固相S与液相L置于高速分散机中，在转速为2000r/min的转速条件下混合搅拌15min即可得到可塑性变形地质聚合物浆料；(c) Take metakaolin as solid phase S, weigh 156.25g liquid phase L and 34.48g metakaolin solid phase S, place solid phase S and liquid phase L in a high-speed disperser, and rotate at a speed of 2000r/min The plastic deformation geopolymer slurry can be obtained by mixing and stirring for 15 minutes under the conditions;
（d）将可塑性变形地质聚合物浆料浇注至20×20×20mm模具，在常温条件下放置30min后脱模，然后进行养护即得到可塑性变形地质聚合物材料。(d) The plastically deformable geopolymer slurry was poured into a 20×20×20 mm mold, placed at room temperature for 30 minutes, and then demolded, and then cured to obtain a plastically deformable geopolymer material.
对常温养护后的可塑性变形地质聚合物材料进行测定，其抗压强度达到60.74Mpa，DSC测试结果表明，所制备的可塑性变形地质聚合物材料的相变温度为63℃。The compressive strength of the plastically deformable geopolymer material after normal temperature curing was measured, and its compressive strength reached 60.74Mpa. The DSC test results showed that the phase transition temperature of the prepared plastically deformable geopolymer material was 63℃.
实施例4：Example 4:
（a）水玻璃溶液的制备：按照每100g的模数为3.31的工业水玻璃称取质量分数96%氢氧化钠28.85g，将称好的工业水玻璃和氢氧化钠进行超声搅拌溶解配成固定模数1.0的水玻璃溶液；(a) Preparation of water glass solution: Weigh 28.85 g of 96% sodium hydroxide by mass per 100 g of industrial water glass with a modulus of 3.31, and dissolve the weighed industrial water glass and sodium hydroxide by ultrasonic stirring to prepare A water glass solution with a fixed modulus of 1.0;
（b）液相L的制备：按照每128.85g的水玻璃溶液称取九水合硅酸钠27.40g，利用搅拌子将称好的水玻璃溶液与九水合硅酸钠进行超声搅拌混合60min、静置4小时后得到液相L；(b) Preparation of liquid phase L: Weigh 27.40 g of sodium silicate nonahydrate per 128.85 g of water glass solution, and use a stirrer to ultrasonically stir and mix the weighed water glass solution and sodium silicate nonahydrate for 60 min. After 4 hours, liquid phase L was obtained;
（c）以偏高岭土为固相S，称取156.25g液相L和0.48g偏高岭土固相S，将固相S与液相L置于高速分散机中，在转速为2000r/min的转速条件下混合搅拌15min即可得到可塑性变形地质聚合物浆料；(c) Using metakaolin as solid phase S, weigh 156.25g liquid phase L and 0.48g metakaolin solid phase S, place solid phase S and liquid phase L in a high-speed disperser, and rotate at a speed of 2000r/min The plastic deformation geopolymer slurry can be obtained by mixing and stirring for 15 minutes under the conditions;
（d）将可塑性变形地质聚合物浆料浇注至20×20×20mm模具，在常温条件下放置30min后脱模，然后进行养护即得到可塑性变形地质聚合物材料。(d) The plastically deformable geopolymer slurry was poured into a 20×20×20 mm mold, placed at room temperature for 30 minutes, and then demolded, and then cured to obtain a plastically deformable geopolymer material.
对常温养护后的可塑性变形地质聚合物材料进行测定，其抗压强度达到0.627Mpa，DSC测试结果表明，所制备的可塑性变形地质聚合物材料的相变温度为55℃。The compressive strength of the plastically deformable geopolymer material after normal temperature curing was measured, and its compressive strength reached 0.627Mpa. The DSC test results showed that the phase transition temperature of the prepared plastically deformable geopolymer material was 55℃.
实施例5：Example 5:
（a）水玻璃溶液的制备：按照每100g的模数为3.31的工业水玻璃称取质量分数96%氢氧化钠28.85g，将称好的工业水玻璃和氢氧化钠进行超声搅拌溶解配成固定模数1.0的水玻璃溶液；(a) Preparation of water glass solution: Weigh 28.85 g of 96% sodium hydroxide by mass per 100 g of industrial water glass with a modulus of 3.31, and dissolve the weighed industrial water glass and sodium hydroxide by ultrasonic stirring to prepare A water glass solution with a fixed modulus of 1.0;
（b）液相L的制备：按照每68.58g的水玻璃溶液称取九水合硅酸钠27.40g，利用搅拌子将称好的水玻璃溶液与九水合硅酸钠进行超声搅拌混合60min、静置4小时后得到液相L；(b) Preparation of liquid phase L: Weigh 27.40 g of sodium silicate nonahydrate per 68.58 g of water glass solution, and use a stirrer to ultrasonically stir and mix the weighed water glass solution and sodium silicate nonahydrate for 60 min. After 4 hours, liquid phase L was obtained;
（c）以偏高岭土为固相S，称取95.98g液相L和32.48g偏高岭土固相S，将固相S与液相L置于高速分散机中，在转速为2000r/min的转速条件下混合搅拌15min即可得到可塑性变形地质聚合物浆料；(c) Using metakaolin as solid phase S, weigh 95.98g liquid phase L and 32.48g metakaolin solid phase S, put solid phase S and liquid phase L in a high-speed disperser, at a speed of 2000r/min The plastic deformation geopolymer slurry can be obtained by mixing and stirring for 15 minutes under the conditions;
（d）将可塑性变形地质聚合物浆料浇注至20×20×20mm模具，在常温条件下放置30min后脱模，然后进行养护即得到可塑性变形地质聚合物材料。(d) The plastically deformable geopolymer slurry was poured into a 20×20×20 mm mold, placed at room temperature for 30 minutes, and then demolded, and then cured to obtain a plastically deformable geopolymer material.
对常温养护后的可塑性变形地质聚合物材料进行测定，其抗压强度达到50.146Mpa，DSC测试结果表明，所制备的可塑性变形地质聚合物材料的相变温度为70℃。The compressive strength of the plastically deformable geopolymer material after normal temperature curing was measured, and its compressive strength reached 50.146Mpa. The DSC test results showed that the phase transition temperature of the prepared plastically deformable geopolymer material was 70℃.
本发明上述实施例方案仅是对本发明的说明而不能限制本发明，权利要求中指出了本发明产品组成成分、成分比例、制备方法参数的范围，而上述的说明并未指出本发明参数的范围，因此，在与本发明的权利要求书相当的含义和范围内的任何改变，都应当认为是包括在权利要求书的范围内。The above-mentioned embodiments of the present invention are only the description of the present invention and cannot limit the present invention. The claims indicate the scope of the composition of the product, the proportion of the components, and the parameters of the preparation method of the present invention, while the above description does not indicate the scope of the parameters of the present invention. Therefore, any changes within the meaning and scope equivalent to the claims of the present invention should be construed as being included in the scope of the claims.
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