CN101633581A - Method for quickly preparing geopolymer material by microwave radiation - Google Patents

Method for quickly preparing geopolymer material by microwave radiation Download PDF

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Publication number
CN101633581A
CN101633581A CN200810132265A CN200810132265A CN101633581A CN 101633581 A CN101633581 A CN 101633581A CN 200810132265 A CN200810132265 A CN 200810132265A CN 200810132265 A CN200810132265 A CN 200810132265A CN 101633581 A CN101633581 A CN 101633581A
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microwave
microwave radiation
solid
minutes
geopolymer
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韩敏芳
贾屹海
李伯涛
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China University of Mining and Technology Beijing CUMTB
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China University of Mining and Technology Beijing CUMTB
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/02Selection of the hardening environment
    • C04B40/0204Selection of the hardening environment making use of electric or wave energy or particle radiation
    • C04B40/0213Electromagnetic waves
    • C04B40/0218Microwaves
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/006Compositions 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
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/10Production of cement, e.g. improving or optimising the production methods; Cement grinding

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  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The invention belongs to the field of inorganic nonmetallic materials, and particularly relates to a method for quickly preparing a geopolymer material by microwave radiation. Raw materials comprise a solid part and a liquid part, and the mass ratio of the solid part to the liquid part is 1/0.1-1/0.7. The solid raw material is mineral and industrial and mining solid wastes containing rich amorphous silicon and aluminum, and the liquid raw material is solution prepared from aqueous solution of caustic alkali and liquid water glass. The invention adopts the technical scheme that all the raw materials for preparing the geopolymer are mixed evenly, injected into a die, sealed by a plastic film and subjected to the microwave radiation. The microwave radiation comprises three steps: firstly, radiating for 1 to 5 minutes in microwave with power of 50 to 100 watts for polymerizing; secondly, radiating for 1 to 10 minutes in microwave with power of 100 to 300 watts for solidifying; and thirdly, radiating for 1 to 3 minutes in microwave with power of 400 to 1,000 watts. After the microwave radiation is finished, the mixture is released from a mold and then placed in natural conditions for several days to form a finished product. The method has the characteristics of high production efficiency, low labor intensity, simple operation and low cost; and the performance of the product is slightly high or not less than that in the prior method.

Description

A kind of method of quickly preparing geopolymer material by microwave radiation
Technical field
The present invention relates to the method that a kind of microwave radiation prepares geology polymer material, belong to field of inorganic nonmetallic material.
Background technology
Geopolymer is mineral polymer, native polymkeric substance, polymkeric substance pottery etc. again, can be widely used as fire-retardant material, high temperature material, gelling material etc.Raw material is mainly the liquid starting material that the solid material that is rich in the sal composition and alkali (K, Na, Cs, Ca) and water glass (K, Na, Cs) are formed, and solid material comprises solid waste and mine tailing, as kaolin, flyash, slag, building waste etc.Temperature of reaction is between 20-150 ℃, and the slip that solid material and liquid starting material are made into solidified in 8-24 hour usually, and 28 days ultimate compression strength can reach 100MPa.This material can replace ordinary Portland cement in some place, also can be used as baking-free ceramic and uses.
Although the set time of geology polymer material is shorter than ordinary Portland cement, usually close with the set time of magnesium cement, but compare with resin class material, still to grow its set time a lot, for some special purposes, be necessary the fast setting method of geologize polymer materials, make it have more widely adaptability to improve material property the set time that shortens material.
In order to improve the speed of reaction of geology polymer material, be necessary to attempt new preparation method, we have proposed to prepare the geology polymeric material with microwave heating method first, and have obtained good material property.
Summary of the invention
The object of the present invention is to provide a kind of microwave radiation to prepare the method for geopolymer, purpose is to improve geopolymeric reaction speed, shortens curing time, enhances productivity, and reduces the production cost of geology polymer material.
Technology official documents and correspondence provided by the invention:
The geopolymer raw material is carried out preheating under microwave radiation, carry out polyreaction, time spent 1-5 minute; Make moisture evaporation through microwave action again, product sclerosis, the demoulding, time spent 1-10 minute; After microwave radiation makes product drying, time spent 1-3 minute.The used microwave power of pre-heating stage is 50-100W, and preheating temperature is controlled between 60-80 ℃; Used microwave power of sclerosis stage is 100-300W, and temperature is controlled between 80-100 ℃; The used microwave power of drying stage is 400-1000W, and temperature is controlled between 100-120 ℃.
According to technical solution of the present invention, all raw materials of preparation geopolymer are made up of two portions, i.e. solid part and liquid portion.Solid part is various mineral, solid waste and the mine tailings etc. that are rich in the sal composition; Liquid portion is the mixture of alkaline solution (K, Na, Cs, Ca) and (K, Na, Cs) sial solution.Wherein the solid part consumption is 40-80% (massfraction), and the liquid portion consumption is 20-60% (massfraction).
Mechanism of the present invention:
Geopolymeric reaction is the reaction between the solid-liquid two-phase, and reaction comprised for four steps: dissolving, diffusion, polymerization and condense.Dissolving and diffusion and temperature relation are close, and the high more dissolving of temperature is fast more, and diffusion is also just fast more.Carry out microwave radiation heating is compared not only the fast but also homogeneous heating of speed with traditional heating mode, system temperature can meet the requirements of temperature at short notice, and this makes the very fast raising of velocity of diffusion, has accelerated polymerization and rate of set, shortened demould time, enhanced productivity.Microwave can also be able to make the solid particulate energy improve, the particle generation depolymerization of reunion, and the solid-liquid contact surface increases, and therefore speed of response also can increase.
The scope of application of the present invention:
The present invention is applicable to that casting and briquetting process prepare geopolymer and composite materials and goods.
Embodiment
Adopting sodium hydroxide, sodium silicate and flyash, standard sand, tap water is raw material, has changed the composition of raw material among the embodiment respectively, and see Table 1 concrete the composition among each embodiment.
Prepared material is a microwave radiation 9 minutes, 12 minutes, 15 minutes in the microwave oven of 700W at power respectively, has contrasted same sample simultaneously at normal temperature (20 ℃) down and 80 ℃ of following maintenances.Tested sample respectively in the ultimate compression strength in the different length of times, the intensity when specifically comprising demoulding, 28 days intensity the results are shown in Table 2-6.
Table 1 embodiment numbering and corresponding raw material are formed
Figure S2008101322651D00021
Embodiment 1: ultimate compression strength increases with the prolongation of microwave time during the sample demoulding, but the intensity in the 28 day length of time is the highest of microwave 12 minutes, reaches 16.3MPa.The intensity of 12 minutes samples of microwave is higher than maintenance under the room temperature, and is lower than 80 ℃ of following maintenances, 21.9MPa.The result is as shown in table 2.
Table 2 embodiment 1---the material ultimate compression strength (MPa) under different maintenance methods and the condition
Figure S2008101322651D00031
Embodiment 2: the same with example 1, the ultimate compression strength of sample increases with the prolongation of microwave time during the demoulding, but the intensity in the 28 day length of time is the highest of microwave 12 minutes, reaches 17.9MPa.The intensity of 12 minutes samples of microwave not only is higher than maintenance under the room temperature, and is higher than 80 ℃ of following maintenances.The result is as shown in table 3.
Table 3 embodiment 2---the material ultimate compression strength (MPa) under different maintenance methods and the condition
Figure S2008101322651D00032
Embodiment 3: the same with 2 with example 1, sample ultimate compression strength increases with the microwave time lengthening during demoulding, and the ultimate compression strength in the 28 day length of time also is the highest of microwave 12 minutes, reaches 12.7MPa.Under the strength ratio room temperature of 12 minutes samples of microwave and 80 ℃ of maintenances all low.The result is as shown in table 4.
Table 4 embodiment 3---the material ultimate compression strength (MPa) under different maintenance methods and the condition
Figure S2008101322651D00041
Embodiment 4: the same with 3 with example 1,2, sample ultimate compression strength increases with the microwave time lengthening during demoulding, but the intensity in the 28 day length of time is the highest of microwave 12 minutes, reaches 16MPa.Under the strength ratio room temperature of 12 minutes samples of microwave and 80 ℃ of maintenances all high.The result is as shown in table 5.
Material ultimate compression strength (MPa) under different maintenance methods of table 5 embodiment 4-and the condition
Figure S2008101322651D00042
Embodiment 5: different with 4 with example 1,2,3, sample ultimate compression strength reduces with the prolongation of microwave time during the demoulding, this may be owing to water content in this sample batching is low, microwave radiation 9 minutes, moisture evaporates away often, radiated time continues to prolong, and is unfavorable for the gain in strength of sample.But the intensity in the 28 day length of time remains the highest of microwave 12 minutes, reaches 6.2MPa.Under the strength ratio room temperature of 12 minutes samples of microwave and 80 ℃ of maintenances all high.The result is as shown in table 6.
Table 6 embodiment 5---the material ultimate compression strength (MPa) under different maintenance methods and the condition
Figure S2008101322651D00051
The The above results explanation, microwave curing helps the raising of goods early strength, and this method especially is fit to require the application places of quick demoulding.Microwave curing 12 minutes, effect is best.

Claims (10)

1, a kind of microwave radiation geopolymer preparation method is characterized by this method and comprises three steps: microwave polymerization, microwave curing and microwave drying.
2, be 50-100W according to the used microwave power of right 1 microwave polymerization, the used time is 1-5 minute.
3, be 100-300W according to the used microwave power of right 1 microwave curing, the used time is 1-10 minute.
4, be 400-1000W according to the used microwave power of right 1 microwave drying, the used time is 1-3 minute.
5, according to right 1,2,3 and 4, polymerization, curing and drying can once be finished, and used microwave power is 400-1000W, and the used time is 3-20 minute.
6, it is two kinds according to the right 1 synthetic used raw material of geopolymer: solid material and liquid starting material.
7, the molding mode according to right 1 preparation geopolymer comprises casting and compression moulding.
8, be mineral and the industry and mining solid waste that is rich in amorphous silicon and aluminium according to right 5 solid materials
9, according to the solution of right 5 liquid starting materials for being made into caustic-alkali aqueous solution and liquid soluble glass.
10, be 1/0.3-1/0.7 according to the solid material of right 6 casting and the ratio of liquid starting material, the solid material of compression moulding and the ratio of liquid starting material are 1/0.1-1/0.3.
CN200810132265A 2008-07-22 2008-07-22 Method for quickly preparing geopolymer material by microwave radiation Pending CN101633581A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633449A (en) * 2012-05-03 2012-08-15 南京大学 High-strength glass base polymer and preparation method thereof
CN105152626A (en) * 2015-10-12 2015-12-16 昊青薪材(北京)技术有限公司 Technology for production of non-sintered ceramic through microwave maintenance of feldspath-quartz tailing
CN105272125A (en) * 2015-09-30 2016-01-27 中国地质大学(武汉) Geopolymer-based rapid repairing material and preparation method thereof
CN110372239A (en) * 2018-04-12 2019-10-25 兴局产业株式会社 Utilize the preparation method of the geo-polymer of the high compressive strength of coal bottom ash
CN110510947A (en) * 2019-08-29 2019-11-29 江苏苏博特新材料股份有限公司 The method that microwave curing prepares the low-quality mine spike recycled cement based articles of large dosage
CN110950680A (en) * 2019-12-27 2020-04-03 广西科学院 Microwave curing method for concrete
CN113603448A (en) * 2021-07-14 2021-11-05 北京荣露材料科技有限公司 Method for preparing green decorative material by utilizing heat-treated and mechanically activated coal gangue

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CN101182168A (en) * 2007-11-27 2008-05-21 中国矿业大学(北京) Lightweight heat insulating material and method for making same

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CN101182168A (en) * 2007-11-27 2008-05-21 中国矿业大学(北京) Lightweight heat insulating material and method for making same

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102633449A (en) * 2012-05-03 2012-08-15 南京大学 High-strength glass base polymer and preparation method thereof
CN105272125A (en) * 2015-09-30 2016-01-27 中国地质大学(武汉) Geopolymer-based rapid repairing material and preparation method thereof
CN105152626A (en) * 2015-10-12 2015-12-16 昊青薪材(北京)技术有限公司 Technology for production of non-sintered ceramic through microwave maintenance of feldspath-quartz tailing
CN110372239A (en) * 2018-04-12 2019-10-25 兴局产业株式会社 Utilize the preparation method of the geo-polymer of the high compressive strength of coal bottom ash
CN110510947A (en) * 2019-08-29 2019-11-29 江苏苏博特新材料股份有限公司 The method that microwave curing prepares the low-quality mine spike recycled cement based articles of large dosage
CN110950680A (en) * 2019-12-27 2020-04-03 广西科学院 Microwave curing method for concrete
CN110950680B (en) * 2019-12-27 2021-07-16 广西科学院 Microwave curing method for concrete
CN113603448A (en) * 2021-07-14 2021-11-05 北京荣露材料科技有限公司 Method for preparing green decorative material by utilizing heat-treated and mechanically activated coal gangue

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Application publication date: 20100127