CN109020378A - A kind of expanded perlite aeroge composite insulation boards and preparation method thereof prepared using iron tailings as raw material - Google Patents

A kind of expanded perlite aeroge composite insulation boards and preparation method thereof prepared using iron tailings as raw material Download PDF

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CN109020378A
CN109020378A CN201810987697.4A CN201810987697A CN109020378A CN 109020378 A CN109020378 A CN 109020378A CN 201810987697 A CN201810987697 A CN 201810987697A CN 109020378 A CN109020378 A CN 109020378A
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iron tailings
expanded perlite
insulation boards
composite insulation
raw material
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CN109020378B (en
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王建国
宋鑫
包志康
杨骏
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
    • C04B28/04—Portland 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
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
    • C04B14/06—Quartz; Sand
    • C04B14/064—Silica aerogel
    • 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
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B18/04—Waste materials; Refuse
    • C04B18/12—Waste materials; Refuse from quarries, mining or the like
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/02—Treatment
    • C04B20/023—Chemical treatment
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/08—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by adding porous substances
    • 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
    • C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
    • 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

Abstract

A method of expanded perlite aeroge composite insulation boards are prepared by raw material of iron tailings, the following steps are included: iron tailings slag, ordinary portland cement, cellulose, rubber powder, short-fibre silk, expanded perlite and hydrophobic silica aerogel powder are mixed, it adds water and stirs uniformly, after forming starchy mixture, it pours into mold, and the embedded fiber grid cloth in the starchy mixture, natural air drying, demoulding is to get expanded perlite aeroge composite insulation boards.Present invention introduces hydrophobic silica aerogels made from the element silicon extracted from iron tailings, so that heat preservation plate material has lower thermal coefficient, and this solid waste of iron tailings slag is largely used, the composite insulation boards that can be mass produced are manufactured that while alleviating environmental pressure.Composite insulation boards produced by the present invention have many advantages, such as low density, good effect of heat insulation, do not burn.The density of the composite insulation boards of preparation is lower than 0.332g/cm3, thermal coefficient be lower than 0.056 w/mK.

Description

A kind of expanded perlite aeroge composite insulation boards prepared using iron tailings as raw material and Preparation method
Technical field
The invention belongs to technical field of inorganic material, and in particular to a kind of expanded perlite prepared using iron tailings as raw material Aeroge composite insulation boards and preparation method thereof.
Background technique
Iron tailings is the solid waste of steel and iron industry discharge.The stockpiling of iron tailings not only occupied cultivated land, pollutes environment, but also needed A large amount of fund is put into go to safeguard.Therefore the comprehensive utilization of research iron tailings is particularly significant.Wherein iron tailings mainly by siliceous and For irony at being grouped as, impurity content is lower, their conventional recovery methods complex process, energy consumption is high, at high cost.
Silica aerogel material is one of insulating solid material best in the world, and is had highest fire-retardant etc. Still, aeroge ultimate tensile strength very little, matter is crisp for grade, frangible, to avoid direct mechanical impact.Due to its structure itself Defect, aerogel products are difficult directly to apply as commodity at present, need and other materials are used in combination.
The insulation board under technology mainly has inorganic/organic two major classes at present, wherein inorganic heat-insulation board such as calcium silicate board, foam It is higher that glass plate etc. is primarily present thermal coefficient, causes plate integral heat insulation performance poor, and insulation board density is higher, is unfavorable for Construction and transport；Although the density such as organic heat-insulating plate such as polyurethane foam board are small, heat insulation effect is good, since it is flammable, The stage of limitation application is still belonged in fields such as buildings.Low thermal conductivity, low-density, higher mechanical strength, tool were both possessed at present There is noninflammability, and the insulation board that can also consume this solid waste of iron tailings on a large scale is not yet reported that.
In view of the above-mentioned problems, prepare hydrophobic silica aerogel using iron tailings as raw material, later and expanded perlite And mine tailings etc. are compound prepares composite insulation boards, and this waste resource of iron tailings is recycled again, is led reaching lower Its mechanical performance is significantly enhanced while hot coefficient, may be directly applied to the fields such as industry, building.
Summary of the invention
For above-mentioned technical problem of the existing technology, the purpose of the present invention is to provide one kind using iron tailings as raw material The heat insulation effect of expanded perlite aeroge composite insulation boards of preparation and preparation method thereof, insulation board prepared by the present invention is good, The advantages that mechanical strength is big, and preparation condition is mild, is easy to industrialize.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In by iron tailings slag, ordinary portland cement, cellulose, rubber powder, short-fibre silk, expanded perlite and hydrophobic silica airsetting The mixing of rubber powder end, adds water and stirs uniformly, after forming starchy mixture, pours into mold, and in the starchy mixing Embedded fiber grid cloth in object, natural air drying demould to get expanded perlite aeroge composite insulation boards.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In by weight, comprising the following steps: by 20 ~ 60 parts of iron tailings slag, 70 ~ 100 parts of ordinary portland cement, cellulose 5 ~ 8 Part, 8 ~ 12 parts of rubber powder, 3 ~ 5 parts of short-fibre silk, 15 ~ 25 parts and 12 ~ 16 parts of hydrophobic silica aerogel powder of expanded perlite Mixing is added water and stirred uniformly, after forming starchy mixture, is poured into mold, and embedding in the starchy mixture Enter 3 ~ 8 parts of fibrous mesh cloth, natural air drying demoulds to get expanded perlite aeroge composite insulation boards.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist It is in the preparation method of the iron tailings slag and hydrophobic silica aerogel powder, comprising the following steps:
1) iron tailings powder is mixed with sodium hydrate particle, is heated to keeping 2 ~ 3 to carry out alkali soluble at 400 ~ 500 DEG C in Muffle furnace Reaction, is cooled to room temperature, and mixture after cooling is mixed with water, heating stirring, and filtering, filter residue and drying is up to the iron tailings Slag, filtrate are collected to get thick silicon solution；
2) after mixing, pouring into aqueous hydrochloric acid solution to pH value is 2 ~ 4 for thick silicon solution and water glass solution obtained by step 1), is stirred It mixes 10 ~ 20min to be fully hydrolyzed, it is 7 ~ 8 that dilute ammonia solution is added dropwise into the mixed liquor after hydrolysis and is adjusted to pH value, is stood to be formed Blocky gel, the aging 20-40min under 40-50 DEG C of bath temperature, obtains wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2,1 ~ 2h of deionized water agitator treating is added, filters, filter residue immerses dehydrated alcohol 0.5 ~ 1.5h of middle stirring carries out exchange of solvent, then is filtered, and filter residue, which immerses, stirs 0.5 ~ 1h in modification liquid, obtains modified mixing Liquid；
4) by modified mixed liquor stratification obtained by step 3), upper liquid is taken to be immersed in 20 ~ 40min of agitator treating in n-hexane, It is filtered, after filter residue carries out constant pressure and dry, is placed in Muffle furnace and roasts 1 ~ 2h at 450 ~ 550 DEG C to get described hydrophobic Silica aerogel powder.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In step 1), the mesh number of iron tailings powder is 100 mesh or more；The ingredient of the iron tailings includes SiO2, CaO, MgO, Al2O3 And Fe2O3.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In step 1), the mass ratio of iron tailings powder and sodium hydrate particle is 1: 1.3 ~ 2.1；The mixture after cooling The ratio of quality and the volume of water is 1: 3 ~ 6, and the unit of quality is g, and the unit of volume is mL；The temperature of heating stirring be 70 ~ 85℃。
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In step 2, the volume ratio of thick silicon solution and water glass solution is 7 ~ 9:1；The concentration of aqueous hydrochloric acid solution is 1 ~ 3mol/L, excellent Select 2mol/L；The concentration of dilute ammonia solution is 0.2 ~ 0.6mol/L, preferably 0.4 mol/L.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In step 3), the quality of the wet colloidal sol after pulverizing is 1:1.2 ~ 2.5 with the volume ratio with deionized water；Filter residue immerses anhydrous second When stirring in alcohol, the quality of filter residue and the volume ratio of dehydrated alcohol are 1:0.9 ~ 1.4；The unit of quality is g, and the unit of volume is mL。
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In step 3), the mixed liquor that modification liquid is made of n-hexane and trim,ethylchlorosilane, n-hexane and front three in the modification liquid The volume ratio of base chlorosilane is 8 ~ 12: 1, preferably 10: 1；Filter residue immerses in modification liquid when stirring, the quality of filter residue with change Property liquid volume ratio be 1:1 ~ 1.5, the unit of quality is g, and the unit of volume is mL.
A kind of method preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, feature exist In step 4), the volume ratio of liquid and n-hexane is 1:0.5 ~ 1 at the middle and upper levels；The temperature of constant pressure and dry be 50 ~ 60 DEG C, the time be 0.5 ~ 1h。
A kind of expanded perlite aeroge composite insulation boards prepared using iron tailings as raw material.
Compared with the existing technology, what the present invention obtained has the beneficial effect that:
1) present invention has rationally recycled the valuable element in tailing, and is handled again remaining waste material, and whole iron have been reached The effective use of tailing.
2) expanded perlite aeroge composite insulation boards prepared by the present invention, have both heat-insulating and fire-proof performance and stronger machinery Intensity overcomes the disadvantage that aerosil matter is crisp, frangible.Hydrophobic silica aerogel and expansion are introduced in insulation board Perlite, aerosil have extremely low thermal coefficient, substantially reduce the thermal coefficient and density of insulation board entirety；Draw Entering tailing waste residue can be enhanced the compression strength of insulation board；Rubber powder, cellulose, fibrous mesh cloth, which is added, can be enhanced insulation board Tension and flexural strength.
3) the present invention provides a kind of methods for preparing expanded perlite aeroge insulation board as raw material using iron tailings, including After being reacted by alkali soluble, the element silicon extracted in iron tailings is mixed with water and obtains cheap silicon source；By deionized water to gel pore A large amount of existing inorganic salts in road are washed, it is easier to carry out the modified operation in surface；Exchange of solvent is carried out to gel And the modified operation in surface, it can be dried to obtain hydrophobic silica aerogel under normal pressure, obtained aerogel powder incorporation Low thermal conductivity is achieved the effect that in expanded perlite plate.
4) expanded perlite aeroge composite insulation boards prepared by the present invention have achieved the effect that lightweight, heat preservation, non-ignitable, Cure stage only needs room temperature maintenance that solidification can be realized without high temperature sintering, can substantially reduce production cost, be easy to work Industry.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the SEM figure that hydrophobic silica aerogel powder is made in present example 1；
Fig. 3 is the structural schematic diagram that expanded perlite aeroge composite insulation boards are made in present example 1.
Specific embodiment
The present invention is further explained in the light of specific embodiments, but the scope of protection of the present invention is not limited thereto.
In the following examples and comparative examples:
The constituent mass percentage composition of iron tailings is as follows: SiO245.43%、CaO 13.81%、MgO 13.10%、Al2O3 11.35%、Fe2O310.13%, surplus is impurity；
The concentration of water glass solution is the aqueous solution that 25% ~ 27%(water glass solution is sodium metasilicate)；
The strength grade of ordinary portland cement is 42.5；Cellulose is hydroxymethyl cellulose；Short-fibre silk is polypropylene fibre Silk；Rubber powder is purchased from Nanchang Yu Sidun construction material Co., Ltd；
The unit of quality is g, and the unit of volume is mL.
Embodiment 1:
A method of expanded perlite aeroge composite insulation boards being prepared by raw material of iron tailings, by weight, including with Lower step:
20 parts of iron tailings slag, 70 parts of ordinary portland cement, 5 parts of cellulose, 8 parts of rubber powder, 3 parts of short-fibre silk, expanded perlite 7 Part, 12 parts of hydrophobic silica aerogel powder mixing, add water and stir uniformly, after forming starchy mixture, pour into mold In, and 3 parts of embedded fiber grid cloth in the starchy mixture, natural air drying is multiple to get expanded perlite aeroge Close insulation board；
The preparation method of above-mentioned iron tailings slag and hydrophobic silica aerogel powder is, comprising the following steps:
1) iron tailings crushes, and the iron tailings powder 1:1.3 in mass ratio that mesh number is 100 mesh or more is taken to mix with sodium hydrate particle It closes, is heated to keeping 2h that alkali soluble reaction occurs at 400 DEG C in Muffle furnace, be cooled to room temperature, mixture after cooling and water are mixed Close by solid-to-liquid ratio be 1:3 mixed (iron tailings i.e. after cooling is mixed with the whole mixt of sodium hydroxide with water, Gu The unit of liquor ratio is g/mL), the heating stirring 12h at 70 DEG C is filtered, and filter residue and drying is collected up to the iron tailings slag, filtrate, Up to thick silicon solution；
2) according to volume ratio 7:1, (water glass solution is added is thick silicon solution obtained by step 1) after mixing with water glass solution To supplement silicon source), pouring into the aqueous hydrochloric acid solution of 2mol/L to pH value is 2, and stirring 10min is fully hydrolyzed, to mixed after hydrolysis It is 7 that the dilute ammonia solution that 0.4mol/L is added dropwise in conjunction liquid, which is adjusted to pH value, blocky gel to be formed is stood, then at 40 DEG C of water-bath At a temperature of aging 20min, obtain wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2, the deionized water (ratio of the volume of the quality and deionized water of wet colloidal sol is added For 1:1.2), agitator treating 1h, filter, filter residue immerse stirring 0.5h in dehydrated alcohol carry out exchange of solvent (quality of filter residue with The volume ratio of dehydrated alcohol is 1:0.9), then filtered, filter residue immerses modification liquid described in stirring 0.5h(in modification liquid and is positive oneself Alkane and the trim,ethylchlorosilane mixed liquor that 10:1 is constituted by volume, the quality of filter residue and the volume ratio of modification liquid are 1:1), it obtains Modified mixed liquor；
4) by modified mixed liquor stratification obtained by step 3), taking upper liquid, 1:0.5 is immersed in n-hexane and stirs by volume 20min is washed, is filtered, filter residue after constant pressure and dry 0.5h, be placed in Muffle furnace and roast at 550 DEG C at 50 DEG C 2h is to get the hydrophobic silica aerogel powder, the surface hydrophilic of the hydrophobic silica aerogel powder, inside It is hydrophobic.
Electron microscope (SEM) analytical table is scanned to hydrophobic silica aerogel powder made from the present embodiment Sign, as a result as shown in Figure 2；From figure 2 it can be seen that the aeroge surface and inside have been covered with nanoscale duct, and siliceous three Tieing up network structure is connected with each other by the uniform particle of particle diameter distribution, and typical aerosil structure is belonged to.Hole Road is evenly distributed and intensively, also its provable high porosity and the reason of low-density.
Embodiment 2:
A method of expanded perlite aeroge composite insulation boards being prepared by raw material of iron tailings, by weight, including with Lower step:
60 parts of iron tailings slag, 100 parts of ordinary portland cement, 8 parts of cellulose, 12 parts of rubber powder, 5 parts of short-fibre silk, expanded pearlite 9 parts of rock, 16 parts of hydrophobic silica aerogel powder mixing, add water and stir uniformly, after forming starchy mixture, pour into mould In tool, and 8 parts of embedded fiber grid cloth in the starchy mixture, natural air drying is to get expanded perlite aeroge Composite insulation boards；
The preparation method of above-mentioned iron tailings slag and hydrophobic silica aerogel powder is, comprising the following steps:
1) iron tailings crushes, and the iron tailings powder 1:2.1 in mass ratio that mesh number is 100 mesh or more is taken to mix with sodium hydrate particle It closes, is heated to keeping 3h that alkali soluble reaction occurs at 500 DEG C in Muffle furnace, be cooled to room temperature, mixture after cooling and water are mixed Closing by solid-to-liquid ratio is that 1:6 is mixed (unit of solid-to-liquid ratio is g/mL), the heating stirring 12h at 85 DEG C, filtering, filter residue is done The dry iron tailings slag to obtain the final product, filtrate are collected to get thick silicon solution；
2) according to volume ratio 9:1, (water glass solution is added is thick silicon solution obtained by step 1) after mixing with water glass solution To supplement silicon source), pouring into the aqueous hydrochloric acid solution of 2mol/L to pH value is 4, and stirring 20min is fully hydrolyzed, to mixed after hydrolysis It is 8 that the dilute ammonia solution that 0.4mol/L is added dropwise in conjunction liquid, which is adjusted to pH value, blocky gel to be formed is stood, then at 50 DEG C of water-bath At a temperature of aging 40min, obtain wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2, the deionized water (ratio of the volume of the quality and deionized water of wet colloidal sol is added For 1:2.5), agitator treating 2h, filter, filter residue immerse stirring 1.5h in dehydrated alcohol carry out exchange of solvent (quality of filter residue with The volume ratio of dehydrated alcohol is 1:1.4), then filtered, filter residue, which immerses in modification liquid, stirs modification liquid described in 1h(as n-hexane With the trim,ethylchlorosilane mixed liquor that 10:1 is constituted by volume, the quality of filter residue and the volume ratio of modification liquid are 1:1.5), it obtains Modified mixed liquor；
4) by modified mixed liquor stratification obtained by step 3), taking upper liquid, 1:1 is immersed in stirring in n-hexane and washes by volume 40min is washed, is filtered, filter residue after constant pressure and dry 1h, be placed in Muffle furnace at 60 DEG C and roast 1h at 450 DEG C, i.e., Obtain the hydrophobic silica aerogel powder, the surface hydrophilic of the hydrophobic silica aerogel powder, inner hydrophobic.
Embodiment 3:
A method of expanded perlite aeroge composite insulation boards being prepared by raw material of iron tailings, by weight, including with Lower step:
30 parts of iron tailings slag, 80 parts of ordinary portland cement, 6 parts of cellulose, 10 parts of rubber powder, 4 parts of short-fibre silk, expanded perlite 8 parts, 15 parts of hydrophobic silica aerogel powder mixing, add water and stir uniformly, after forming starchy mixture, pour into mold In, and 5 parts of embedded fiber grid cloth in the starchy mixture, natural air drying is multiple to get expanded perlite aeroge Close insulation board；
The preparation method of above-mentioned iron tailings slag and hydrophobic silica aerogel powder is, comprising the following steps:
1) iron tailings crushes, and the iron tailings powder 1:1.6 in mass ratio that mesh number is 100 mesh or more is taken to mix with sodium hydrate particle It closes, is heated to keeping 2.5h that alkali soluble reaction occurs at 450 DEG C in Muffle furnace, be cooled to room temperature, mixture and water after cooling Mixing is that 1:4 is mixed (unit of solid-to-liquid ratio is g/mL) by solid-to-liquid ratio, the heating stirring 12h at 80 DEG C, filtering, filter residue It is drying to obtain the iron tailings slag, filtrate is collected to get thick silicon solution；
2) according to volume ratio 7:1, (water glass solution is added is thick silicon solution obtained by step 1) after mixing with water glass solution To supplement silicon source), pouring into the aqueous hydrochloric acid solution of 2mol/L to pH value is 3, and stirring 15min is fully hydrolyzed, to mixed after hydrolysis It is 7.5 that the dilute ammonia solution that 0.4mol/L is added dropwise in conjunction liquid, which is adjusted to pH value, blocky gel to be formed is stood, then at 45 DEG C of water Aging 30min under bath temperature obtains wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2, the deionized water (ratio of the volume of the quality and deionized water of wet colloidal sol is added For 1:1.6), agitator treating 1.5h, filter, filter residue immerse stirring 1h in dehydrated alcohol carry out exchange of solvent (quality of filter residue with The volume ratio of dehydrated alcohol is 1:1), then filtered, filter residue immerse in modification liquid stir modification liquid described in 1h(be n-hexane with The trim,ethylchlorosilane mixed liquor that 10:1 is constituted by volume, the quality of filter residue and the volume ratio of modification liquid are 1:1.2), it must change Property mixed liquor；
4) by modified mixed liquor stratification obtained by step 3), taking upper liquid, 1:0.9 is immersed in n-hexane and stirs by volume 30min is washed, is filtered, filter residue after constant pressure and dry 1h, be placed in Muffle furnace and roast at 500 DEG C at 55 DEG C 1.5h is the surface hydrophilic of the hydrophobic silica aerogel powder, interior to get the hydrophobic silica aerogel powder Portion is hydrophobic.
Embodiment 4:
A method of expanded perlite aeroge composite insulation boards being prepared by raw material of iron tailings, by weight, including with Lower step:
50 parts of iron tailings slag, 80 parts of ordinary portland cement, 7 parts of cellulose, 10 parts of rubber powder, 5 parts of short-fibre silk, expanded perlite 8 parts, 15 parts of hydrophobic silica aerogel powder mixing, add water and stir uniformly, after forming starchy mixture, pour into mold In, and 6 parts of embedded fiber grid cloth in the starchy mixture, natural air drying is multiple to get expanded perlite aeroge Close insulation board；
The preparation method of above-mentioned iron tailings slag and hydrophobic silica aerogel powder is, comprising the following steps:
1) iron tailings crushes, and the iron tailings powder 1:1.7 in mass ratio that mesh number is 100 mesh or more is taken to mix with sodium hydrate particle It closes, is heated to keeping 2.5h that alkali soluble reaction occurs at 480 DEG C in Muffle furnace, be cooled to room temperature, mixture and water after cooling Mixing is that 1:5 is mixed (unit of solid-to-liquid ratio is g/mL) by solid-to-liquid ratio, the heating stirring 12h at 80 DEG C, filtering, filter residue It is drying to obtain the iron tailings slag, filtrate is collected to get thick silicon solution；
2) according to volume ratio 8:1, (water glass solution is added is thick silicon solution obtained by step 1) after mixing with water glass solution To supplement silicon source), pouring into the aqueous hydrochloric acid solution of 2mol/L to pH value is 3, and stirring 16min is fully hydrolyzed, to mixed after hydrolysis It is 8 that the dilute ammonia solution that 0.4mol/L is added dropwise in conjunction liquid, which is adjusted to pH value, blocky gel to be formed is stood, then at 50 DEG C of water-bath At a temperature of aging 30min, obtain wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2, the deionized water (ratio of the volume of the quality and deionized water of wet colloidal sol is added It for 1:1.8), agitator treating 2h, filters, filter residue immerses stirring 1h in dehydrated alcohol and carries out the exchange of solvent (quality and nothing of filter residue The volume ratio of water-ethanol is 1:1.2), then filtered, filter residue immerse in modification liquid stir modification liquid described in 1h(be n-hexane with The trim,ethylchlorosilane mixed liquor that 10:1 is constituted by volume, the quality of filter residue and the volume ratio of modification liquid are 1:1.4), it must change Property mixed liquor；
4) by modified mixed liquor stratification obtained by step 3), taking upper liquid, 1:1 is immersed in stirring in n-hexane and washes by volume 35min to be washed, is filtered, filter residue after constant pressure and dry 1h, be placed in Muffle furnace at 60 DEG C and roast 1.5h at 520 DEG C, Up to the hydrophobic silica aerogel powder, the surface hydrophilic of the hydrophobic silica aerogel powder, inside are dredged Water.
Comparative example 1:
A method of expanded perlite aeroge composite insulation boards being prepared by raw material of iron tailings, by weight, including with Lower step:
20 parts of iron tailings slag, 70 parts of ordinary portland cement, 5 parts of cellulose, 8 parts of rubber powder, 3 parts of short-fibre silk, expanded perlite 7 Part, 12 parts of hydrophobic silica aerogel powder mixing, add water and stir uniformly, after forming starchy mixture, pour into mold In, and 3 parts of embedded fiber grid cloth in the starchy mixture, natural air drying is multiple to get expanded perlite aeroge Close insulation board；
The preparation method of above-mentioned iron tailings slag and hydrophobic silica aerogel powder is, by identical inventory in embodiment 1 into Row comparison, comprising the following steps:
1) iron tailings crushes, and the iron tailings powder 1:1.3 in mass ratio that mesh number is 100 mesh or more is taken to mix with sodium hydrate particle It closes, is heated to keeping 2h that alkali soluble reaction occurs at 400 DEG C in Muffle furnace, be cooled to room temperature, mixture after cooling and water are mixed Close by solid-to-liquid ratio be 1:3 mixed (iron tailings i.e. after cooling is mixed with the whole mixt of sodium hydroxide with water, Gu The unit of liquor ratio is g/mL), the heating stirring 12h at 70 DEG C is filtered, and filter residue and drying is collected up to the iron tailings slag, filtrate, Up to thick silicon solution；
2) thick silicon solution obtained by step 1) according to volume ratio 7:1 and deionized water after mixing, pour into the hydrochloric acid water of 2mol/L In solution to pH value be 2, stirring 10min be fully hydrolyzed, the weak aqua ammonia that 0.4mol/L is added dropwise into the mixed liquor after hydrolysis is molten It is 7 that liquid, which is adjusted to pH value, stands blocky gel to be formed, and the aging 20min under 40 DEG C of bath temperature obtains wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2, the deionized water (ratio of the volume of the quality and deionized water of wet colloidal sol is added For 1:1.2), agitator treating 1h, filter, filter residue immerse stirring 0.5h in dehydrated alcohol carry out exchange of solvent (quality of filter residue with The volume ratio of dehydrated alcohol is 1:0.9), then filtered, filter residue immerses modification liquid described in stirring 0.5h(in modification liquid and is positive oneself Alkane and the trim,ethylchlorosilane mixed liquor that 10:1 is constituted by volume, the quality of filter residue and the volume ratio of modification liquid are 1:1), it obtains Modified mixed liquor；
4) by modified mixed liquor stratification obtained by step 3), taking upper liquid, 1:0.5 is immersed in n-hexane and stirs by volume 20min is washed, is filtered, filter residue after constant pressure and dry 0.5h, be placed in Muffle furnace and roast at 550 DEG C at 50 DEG C 2h is to get the hydrophobic silica aerogel powder, the surface hydrophilic of the hydrophobic silica aerogel powder, inside It is hydrophobic.
Comparative example 2:
A method of expanded perlite aeroge composite insulation boards being prepared by raw material of iron tailings, by weight, including with Lower step:
20 parts of iron tailings slag, 70 parts of ordinary portland cement, 5 parts of cellulose, 8 parts of rubber powder, 3 parts of short-fibre silk, expanded perlite 7 Part, 12 parts of hydrophobic silica aerogel powder mixing, add water and stir uniformly, after forming starchy mixture, pour into mold In, and 3 parts of embedded fiber grid cloth in the starchy mixture, natural air drying is multiple to get expanded perlite aeroge Close insulation board；
The preparation method of above-mentioned iron tailings slag and hydrophobic silica aerogel powder is, by identical inventory in embodiment 1 into Row comparison, comprising the following steps:
1) by deionized water according to volume ratio 7:1 and water glass solution after mixing, pour into the aqueous hydrochloric acid solution of 2mol/L It is 2 to pH value, stirring 10min is fully hydrolyzed, and the dilute ammonia solution that 0.4mol/L is added dropwise into the mixed liquor after hydrolysis is adjusted to PH value is 7, stands blocky gel to be formed, and the aging 20min under 40 DEG C of bath temperature obtains wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2, the deionized water (ratio of the volume of the quality and deionized water of wet colloidal sol is added For 1:1.2), agitator treating 1h, filter, filter residue immerse stirring 0.5h in dehydrated alcohol carry out exchange of solvent (quality of filter residue with The volume ratio of dehydrated alcohol is 1:0.9), then filtered, filter residue immerses modification liquid described in stirring 0.5h(in modification liquid and is positive oneself Alkane and the trim,ethylchlorosilane mixed liquor that 10:1 is constituted by volume, the quality of filter residue and the volume ratio of modification liquid are 1:1), it obtains Modified mixed liquor；
4) by modified mixed liquor stratification obtained by step 3), taking upper liquid, 1:0.5 is immersed in n-hexane and stirs by volume 20min is washed, is filtered, filter residue after constant pressure and dry 0.5h, be placed in Muffle furnace and roast at 550 DEG C at 50 DEG C 2h is to get the hydrophobic silica aerogel powder, the surface hydrophilic of the hydrophobic silica aerogel powder, inside It is hydrophobic.
The hydrophobic silica aerogel powder prepared to embodiment 1 ~ 4 and comparative example 1 ~ 2 is tested for the property, and detects it Tap density and porosity, testing result are as shown in table 1；The insulation board prepared to embodiment 1 ~ 4 and comparative example 1 ~ 2 carries out performance Test, detects its density and total thermal coefficient, testing result is as shown in table 1；The examination criteria of tap density is GB/T in table 1 21354-2008, the examination criteria of total thermal coefficient are GB/T 10295.The examination criteria of insulation board density is JC/T990- 2006。
Table 1
Grouping Aeroge porosity Aeroge tap density Insulation board density The total thermal coefficient of insulation board
Embodiment 1 94% 0.168g/cm3 0.332 g/cm3 0.056w/m·K
Embodiment 2 94% 0.166g/cm3 0.317g/cm3 0.052w/m·K
Embodiment 3 94% 0.150g/cm3 0.318g/cm3 0.050w/m·K
Embodiment 4 93% 0.159g/cm3 0.324g/cm3 0.051w/m·K
Comparative example 1 77% 0.507g/cm3 0.358g/cm3 0.064w/m·K
Comparative example 2 80% 0.461g/cm3 0.370g/cm3 0.062w/m·K
As can be drawn from Table 1, aerogel products density obtained by comparative example 1 ~ 2 is larger, and porosity is lower.This is because this is Due to, that water glass solution is not added, carrying out silicon source supplement to thick silicon solution in comparative example 1, the gel for causing it to be formed is softer, Mesh skeleton is relatively fine, in the drying process since the surface tension of solvent causes duct to collapse, finally formed aerogel Product contraction is larger, and density is higher, is not belonging to the range of aeroge；That thick silicon solution is not added in comparative example 2, and waterglass is dilute It releases that ratio is excessively high, causes to only form the gel that matter is soft, skeleton is thin, structure collapse leads to volume contraction hole in the drying process Rate reduces, this has turned out the present invention and has extracted more element silicon in the reaction of iron tailings powder alkali soluble, and illustrates thick silicon solution It mixes and is necessary with a small amount of water glass solution.
As it can be seen from table 1 since the performance of the aeroge of incorporation is poor, insulation board density obtained by comparative example 1 ~ 2 Larger and total thermal coefficient is higher, not only influences usage experience, but also heat insulation effect is poor.
Content described in this specification is only to enumerate to inventive concept way of realization, and protection scope of the present invention is not answered When the concrete form for being seen as limited by embodiment and being stated, protection scope of the present invention is also only in those skilled in the art's root According to present inventive concept it is conceivable that equivalent technologies mean.

Claims (10)

1. a kind of method for preparing expanded perlite aeroge composite insulation boards as raw material using iron tailings, it is characterised in that by iron tail Slag, ordinary portland cement, cellulose, rubber powder, short-fibre silk, expanded perlite and hydrophobic silica aerogel powder are mixed It closes, adds water and stirs uniformly, after forming starchy mixture, pour into mold, and be embedded in the starchy mixture Fibrous mesh cloth, natural air drying demould to get expanded perlite aeroge composite insulation boards.
2. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 1 Method, it is characterised in that by weight, comprising the following steps:
By 20 ~ 60 parts of iron tailings slag, 70 ~ 100 parts of ordinary portland cement, 5 ~ 8 parts of cellulose, 8 ~ 12 parts of rubber powder, short-fibre silk 3 15 ~ 25 parts and 12 ~ 16 parts of hydrophobic silica aerogel powder ~ 5 parts, expanded perlite mixing, add water and stir uniformly, form slurry It after the mixture of paste, pours into mold, and 3 ~ 8 parts of embedded fiber grid cloth in the starchy mixture, natural wind It is dry, it demoulds to get expanded perlite aeroge composite insulation boards.
3. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 1 Method, it is characterised in that the preparation method of the iron tailings slag and hydrophobic silica aerogel powder is, comprising the following steps:
1) iron tailings powder is mixed with sodium hydrate particle, is heated to keeping 2 ~ 3 alkali soluble occurs at 400 ~ 500 DEG C in Muffle furnace Reaction, is cooled to room temperature, and mixture after cooling is mixed with water, heating stirring, and filtering, filter residue and drying is up to the iron tailings Slag, filtrate are collected to get thick silicon solution；
2) after mixing, pouring into aqueous hydrochloric acid solution to pH value is 2 ~ 4 for thick silicon solution and water glass solution obtained by step 1), is stirred It mixes 10 ~ 20min to be fully hydrolyzed, it is 7 ~ 8 that dilute ammonia solution is added dropwise into the mixed liquor after hydrolysis and is adjusted to pH value, is stood to be formed Blocky gel, the aging 20-40min under 40-50 DEG C of bath temperature, obtains wet colloidal sol；
3) after pulverizing wet colloidal sol obtained by step 2,1 ~ 2h of deionized water agitator treating is added, filters, filter residue immerses dehydrated alcohol 0.5 ~ 1.5h of middle stirring carries out exchange of solvent, then is filtered, and filter residue, which immerses, stirs 0.5 ~ 1h in modification liquid, obtains modified mixing Liquid；
4) by modified mixed liquor stratification obtained by step 3), upper liquid is taken to be immersed in 20 ~ 40min of agitator treating in n-hexane, It is filtered, after filter residue carries out constant pressure and dry, is placed in Muffle furnace and roasts 1 ~ 2h at 450 ~ 550 DEG C to get described hydrophobic Silica aerogel powder.
4. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 3 Method, it is characterised in that in step 1), the mesh number of iron tailings powder is 100 mesh or more；The ingredient of the iron tailings includes SiO2、 CaO、MgO、Al2O3And Fe2O3。
5. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 3 Method, it is characterised in that in step 1), the mass ratio of iron tailings powder and sodium hydrate particle is 1: 1.3 ~ 2.1；The cooling The ratio of the volume of the quality and water of mixture afterwards is 1: 3 ~ 6, and the unit of quality is g, and the unit of volume is mL；Heating stirring Temperature be 70 ~ 85 DEG C.
6. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 3 Method, it is characterised in that in step 2, the volume ratio of thick silicon solution and water glass solution is 7 ~ 9:1；The concentration of aqueous hydrochloric acid solution is 1 ~ 3mol/L, preferably 2mol/L；The concentration of dilute ammonia solution is 0.2 ~ 0.6mol/L, preferably 0.4 mol/L.
7. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 3 Method, it is characterised in that in step 3), the quality of the wet colloidal sol after pulverizing and the volume ratio of deionized water are 1:1.2 ~ 2.5；Filter residue When stirring in immersion dehydrated alcohol, the quality of filter residue and the volume ratio of dehydrated alcohol are 1:0.9 ~ 1.4；The unit of quality is g, body Long-pending unit is mL.
8. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 3 Method, it is characterised in that in step 3), the mixed liquor that modification liquid is made of n-hexane and trim,ethylchlorosilane, in the modification liquid just The volume ratio of hexane and trim,ethylchlorosilane is 8 ~ 12: 1, preferably 10: 1；When being stirred in filter residue immersion modification liquid, filter residue Quality and the volume ratio of modification liquid be 1:1 ~ 1.5, the unit of quality is g, and the unit of volume is mL.
9. a kind of side for preparing expanded perlite aeroge composite insulation boards using iron tailings as raw material according to claim 3 Method, it is characterised in that the volume ratio of liquid and n-hexane is 1:0.5 ~ 1 to step 4) at the middle and upper levels；The temperature of constant pressure and dry is 50 ~ 60 DEG C, Time is 0.5 ~ 1h.
10. the expanded perlite aeroge composite insulation boards of any method preparation according to claim 1 ~ 9.
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CN112062519A (en) * 2020-09-03 2020-12-11 北京华阳众信建材有限公司 High-weather-resistance ceramic tile binder and preparation method and construction method thereof
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CN109809789A (en) * 2019-04-01 2019-05-28 浙江工业大学 A method of construction wall thermal insulation clamp central layer is prepared by raw material of silica hydrogel
CN109809790A (en) * 2019-04-01 2019-05-28 浙江工业大学 A kind of insulating brick and preparation method thereof prepared using silica hydrogel as raw material
CN109809789B (en) * 2019-04-01 2021-06-29 浙江工业大学 Method for preparing building wall heat-insulating sandwich layer by taking silicon dioxide hydrogel as raw material
CN109809790B (en) * 2019-04-01 2021-08-03 浙江工业大学 Insulating brick prepared by taking silicon dioxide hydrogel as raw material and preparation method thereof
CN110282933A (en) * 2019-07-26 2019-09-27 浙江工业大学 A kind of microlight-type heat insulation inner core and preparation method thereof prepared using iron tailings powder as raw material
DE112021000806T5 (en) 2020-01-31 2023-01-05 Ondokuz Mayis Universitesi Lightweight foam concrete thermal insulation board and block wall material with infill material inside
CN113563046A (en) * 2020-04-29 2021-10-29 台湾气凝胶科技材料开发股份有限公司 Preparation method of high-temperature-resistant, heat-insulating and fireproof aerogel/inorganic fiber composite adhesive material and application of product thereof
CN113563046B (en) * 2020-04-29 2023-03-14 台湾气凝胶科技材料开发股份有限公司 Preparation method of high-temperature-resistant, heat-insulating and fireproof aerogel/inorganic fiber composite adhesive material and application of product thereof
CN112062519A (en) * 2020-09-03 2020-12-11 北京华阳众信建材有限公司 High-weather-resistance ceramic tile binder and preparation method and construction method thereof

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