CN108892419A - A kind of preparation method of inorganic wall heat-insulating material - Google Patents
A kind of preparation method of inorganic wall heat-insulating material Download PDFInfo
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- CN108892419A CN108892419A CN201810727086.6A CN201810727086A CN108892419A CN 108892419 A CN108892419 A CN 108892419A CN 201810727086 A CN201810727086 A CN 201810727086A CN 108892419 A CN108892419 A CN 108892419A
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- perlite
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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
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/02—Macromolecular compounds
- C04B26/28—Polysaccharides or derivatives thereof
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/34—Non-shrinking or non-cracking materials
- C04B2111/343—Crack resistant materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
-
- 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
-
- 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
Abstract
The present invention relates to a kind of preparation methods of inorganic wall heat-insulating material, belong to construction material preparation technical field.The present invention passes through high-temperature calcination first and perlite is expanded,So that perlite internal void increases,Followed by main component silicon dioxde reaction of sodium hydroxide under conditions of high temperature and pressure and in expanded perlite,Perlite and vegetable oil are blended the present invention,First rancid processing,It is removed so that the organic acid of rancid generation dissolves out ingredient acid-soluble in perlite,Modified perlite and filtrate containing sodium metasilicate and gelatin solution are blended the last present invention,Hydrolysis and condensation polymerization reaction occurs under the action of an acid using sodium metasilicate,Hydrolyze generate silicone hydroxyl in addition to other than self-condensation,Also hydrogen bond action is generated with the hydroxyl activity site of amino and carboxyl and modified pearl rock surface in gelatin,When it is acted on by extraneous stress,Three-dimensional net structure can play the role of dispersive stress,Crack resistence performance is splendid,It has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of inorganic wall heat-insulating material, belong to construction material preparation technical field.
Background technique
Wall heat insulation material（Also known as WW wall heat insulation material）It is both heat-insulated in capable of either internally or externally having for wall
The material of heat insulation function, thermal insulation material product is very more, and most of is all exterior-wall heat insulation, and just insulating layer is done while building
It is good, also there is internal insulation, the stair of general building are all internal insulations.Wall energy-saving and heat-insulating material includes organic（Such as benzene
Plate, styrofoam, extruded sheet, polystyrene foam plate, hard foam polyurethane, polycarbonate and phenolic aldehyde etc.）, inorganic（Such as treasure
Pearl rock cement plate, foamed cement board, composition silicate, rock wool, steam pressure sand aerated concrete block, conventional vacuum mortar etc.）With
Composite material class（Such as metal battenboard, core material are polyphenyl, glass bead, granular polystyrene）, thermal insulative anti-crack material：（Electrowelding net,
Hot-galvanized steel silk screen, grid cloth）.
To promote and apply novel wall material, land resource and ecological environment are protected, energy saving, promotion circular economy hair
Exhibition, many places in China are according to the local practical institution of regulations.Novel wall body heat insulation material enters Rapid development stage, has currently been in
Large-scale development；2001, the dynamics that country further increases superseded traditional material, promotes Novel wall body heat insulation material,
Promoted extension extends to small city, cities and towns, extends to rural area, extends to industrial building.There are building-block, aerated-block, gypsum
Building-block, aerating flyash brick, porous clay brick, GRC wallboard, reinforcing fiber cement plate, battenboard, fly ash aerated wallboard
And composite thermo-insulating wall board, it may be said that many kinds of.
Expanded perlite be another traditional inorganic heat insulation material its be often used as aglite and mix in people's concrete,
To realize the heat insulation effect of wall.Particle of expanded perlite itself have the characteristics that internal porous to its with it is light,
The characteristics of absorbing sound and can be used as thermal insulation material.Thermal coefficient is refractoriness under its high temperature, is a kind of traditional building heat preservation material
Material, application are very extensive.Even so but expanded perlite there is also fatal defects.Its water absorption rate is higher, and absorbs water and hold
It is also easy to produce and expands and the wall temperature change in addition that cracks can make it further generate cracking.
Therefore, a kind of low and not easy to crack inorganic wall heat-insulating material of water absorption rate is invented to lead construction material technology of preparing
Domain has positive effect.
Summary of the invention
Present invention mainly solves the technical issues of, for common expanded perlite class wall heat insulation material water absorption rate at present
Higher, water suction is easy to produce expansion and the wall temperature change in addition that cracks can make it further generate the defect of cracking, provides
A kind of preparation method of inorganic wall heat-insulating material.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that：
A kind of preparation method of inorganic wall heat-insulating material, it is characterised in that specifically preparation step is：
（1）It weighs perlite to be put into high temperature furnace, calcines, obtain expanded perlite, be 30% by expanded perlite and mass fraction
Sodium hydroxide solution mixing after be put into autoclave, seal reaction kettle, high-temperature high-voltage reaction；
（2）To it is above-mentioned after reaction, filtering, respectively obtain filter residue and filtrate, filtrate is spare, repeatedly with deionized water by filter residue
Rinse 3~5 times, then by after flushing filter residue and castor oil mix after obtain mixture, and mixture is put into fermentor；
（3）First above-mentioned fermentor opening is put in the process chamber, stands rancid processing 5~7 days, rancid after treatment, sealing
Fermentation tank mouth, standing for fermentation take out tunning after fermentation to above-mentioned, are put into baking after being rinsed 3~5 times with deionized water
Case, dry 1~2h, obtains modified expanded perlite at 105~110 DEG C；
（4）By mass fraction be 40% gelatin solution and spare filtrate and above-mentioned modified expanded perlite be mixed to get it is mixed
Liquid is closed, pH of mixed is adjusted to 3~5 with the oxalic acid solution that concentration is 1mol/L, is with volume fraction again after standing 1~2h of reaction
1% ammonium hydroxide adjusts pH of mixed to 6~7, the reaction was continued 20~30min；
（5）Reaction product is poured into surface plate after reaction to above-mentioned, still aging 46~48h, is answered at normal temperature
Gel is closed, 8~10h is stood after plural gel and deionized water are mixed, is freeze-dried after standing with vacuum freeze-drying machine, out
Up to inorganic wall heat-insulating material after material.
Step（1）Described in the temperature of calcining be 1000~1300 DEG C, time of calcining is 1~2h, expanded perlite
The mass ratio for the sodium hydroxide solution for being 30% with mass fraction is 1:5, the pressure of high temperature and pressure is 1.5~1.8MPa, and high temperature is high
The temperature of pressure reaction is 150~160 DEG C, 20~30min of time of high-temperature high-voltage reaction.
Step（2）Described in filter residue and castor oil mass ratio be 1:1.
Step（3）Described in process chamber in temperature be 25~35 DEG C, relative air humidity is 65~80%, stand hair
The temperature of ferment is 38~40 DEG C, and the time of standing for fermentation is 5~7 days.
Step（4）Described in gelatin solution and the mass ratio of filtrate and modified expanded perlite be 5:5:1.
Step（5）Described in plural gel and deionized water mass ratio be 1:5.
The beneficial effects of the invention are as follows：
For the present invention first using the perlite with low thermal conductivity as raw material, first high-temperature calcination makes its expansion, then by expanded pearlite
Rock and lye carry out high-temperature high-voltage reaction, respectively obtain reaction filter residue and reaction filtrate, and reaction filter residue and vegetable oil blending are put
Rancid processing under conditions of high temperature and humidity, then rancid product is sealed by fermentation, by fermentation material and filtrate and gelatin cross-blend,
It is reacted under the catalytic action of acid, inorganic wall heat-insulating material is made in final be freeze-dried, and the present invention is made by high-temperature calcination first
Perlite expansion under conditions of high temperature and pressure and expands so that perlite internal void increases followed by sodium hydroxide
Main component silicon dioxde reaction in perlite produces sodium metasilicate and water, further improves expansion after consuming silica
The interior porosity of perlite, and the raising of porosity, it is meant that it can accommodate more air in expanded perlite, and air
It is the non-conductor of heat, therefore the perlite after alkali process has more excellent heat insulation, thermal insulation property is strong, then this hair
It is bright that perlite and vegetable oil are blended, first rancid processing, so that the organic acid of rancid generation is molten by ingredient acid-soluble in perlite
It removes out, further increases its porosity and heat insulation effect, continue to be sealed by fermentation after rancid processing, will be planted by microbial fermentation
Object grease, which is further degraded, generates a large amount of free property ester groups, and these ester groups are introduced into perlite surface and internal void
In, the introducings of these hydrophobicity ester groups will not generate expansion because of water suction and open so that the water absorption rate of perlite is greatly lowered
It splits, modified perlite and filtrate containing sodium metasilicate and gelatin solution are blended the last present invention, are existed using sodium metasilicate
Hydrolysis and condensation polymerization reaction occur under the action of acid, hydrolyze the silicone hydroxyl of generation in addition to other than self-condensation, also and in gelatin
Amino and the hydroxyl activity site on carboxyl and modified pearl rock surface generate hydrogen bond action, gradually form tridimensional network
Gel structure, then be finally made swollen through exchange of solvent and Freeze Drying Technique so that network structure is more stable by ageing
Swollen perlite aeroge makes it have splendid tensile toughness as inorganic wall heat-insulating material, the network structure of aeroge,
When it is acted on by extraneous stress, three-dimensional net structure can play the role of dispersive stress, therefore crack resistence performance is splendid, tool
Have broad application prospects.
Specific embodiment
It weighs perlite to be put into high temperature furnace, is heated to 1000~1300 DEG C, calcine 1~2h, obtain expanded pearlite
The sodium hydroxide solution that expanded perlite and mass fraction are 30% is 1 by rock in mass ratio:Autoclave is put into after 5 mixing
In, reaction kettle is sealed, is heated to 150~160 DEG C under conditions of pressure is 1.5~1.8MPa, high-temperature high-voltage reaction 20
~30min；To it is above-mentioned after reaction, filtering, respectively obtain filter residue and filtrate, filtrate is spare, and filter residue deionized water is anti-
Rinse 3~5 times again, then by after flushing filter residue and castor oil mixed by equal mass ratioes after obtain mixture, and mixture is put
Enter in fermentor；Above-mentioned fermentor opening is first placed on the process chamber that temperature is 25~35 DEG C, relative air humidity is 65~80%
In, rancid processing 5~7 days are stood, rancid after treatment is sealed by fermentation tank mouth, is left to ferment 5 at being 38~40 DEG C in temperature
~7 days, tunning is taken out after fermentation to above-mentioned, baking oven is put into after being rinsed 3~5 times with deionized water, 105~110
Dry 1~2h, obtains modified expanded perlite at DEG C；By mass fraction be 40% gelatin solution and spare filtrate and on
State modified expanded perlite is 5 in mass ratio:5:1 is mixed to get mixed liquor, is adjusted with the oxalic acid solution that concentration is 1mol/L mixed
Liquid pH to 3~5 is closed, adjusts pH of mixed to 6~7 for 1% ammonium hydroxide with volume fraction again after standing 1~2h of reaction, the reaction was continued
20~30min；Reaction product is poured into surface plate after reaction to above-mentioned, still aging 46~48h, obtains at normal temperature
It is in mass ratio 1 by plural gel and deionized water to plural gel:8~10h is stood after 5 mixing, uses vacuum after standing
Freeze dryer freeze-drying, up to inorganic wall heat-insulating material after discharging.
Example 1
It weighs perlite to be put into high temperature furnace, is heated to 1000 DEG C, calcine 1h, expanded perlite is obtained, by expanded pearlite
The sodium hydroxide solution that rock and mass fraction are 30% is 1 in mass ratio:It is put into autoclave after 5 mixing, sealing reaction
Kettle is heated to 150 DEG C under conditions of pressure is 1.5MPa, high-temperature high-voltage reaction 20min；To it is above-mentioned after reaction,
Filtering, respectively obtains filter residue and filtrate, and filtrate is spare, by filter residue with deionized water repeated flushing 3 times, then by the filter residue after flushing
Mixture is obtained after mixing with castor oil by equal mass ratioes, and mixture is put into fermentor；It is first that above-mentioned fermentor is open
It is placed in the process chamber that temperature is 25 DEG C, relative air humidity is 65%, stands rancid processing 5 days, rancid after treatment is close
Seal fermentation tank mouth, temperature be 38 DEG C at be left to ferment 5 days, to it is above-mentioned after fermentation, taking-up tunning, use deionized water
It is put into baking oven after rinsing 3 times, dry 1h, obtains modified expanded perlite at 105 DEG C；The gelatin for being 40% by mass fraction is molten
Liquid and spare filtrate and above-mentioned modified expanded perlite are 5 in mass ratio:5:1 is mixed to get mixed liquor, is with concentration
The oxalic acid solution of 1mol/L adjusts pH of mixed to 3, adjusts mixed liquor with the ammonium hydroxide that volume fraction is 1% again after standing reaction 1h
PH to 6, the reaction was continued 20min；Reaction product is poured into surface plate after reaction to above-mentioned, it is still aging at normal temperature
46h obtains plural gel, is in mass ratio 1 by plural gel and deionized water:8h is stood after 5 mixing, is used after standing true
Empty freeze dryer freeze-drying, up to inorganic wall heat-insulating material after discharging.
Example 2
It weighs perlite to be put into high temperature furnace, is heated to 1150 DEG C, calcine 1.5h, obtain expanded perlite, expansion is precious
The sodium hydroxide solution that Zhu Yan and mass fraction are 30% is 1 in mass ratio:It is put into autoclave after 5 mixing, sealing reaction
Kettle is heated to 155 DEG C under conditions of pressure is 1.7MPa, high-temperature high-voltage reaction 25min；To it is above-mentioned after reaction,
Filtering, respectively obtains filter residue and filtrate, and filtrate is spare, by filter residue with deionized water repeated flushing 4 times, then by the filter residue after flushing
Mixture is obtained after mixing with castor oil by equal mass ratioes, and mixture is put into fermentor；It is first that above-mentioned fermentor is open
It is placed in the process chamber that temperature is 30 DEG C, relative air humidity is 70%, stands rancid processing 6 days, rancid after treatment is close
Seal fermentation tank mouth, temperature be 39 DEG C at be left to ferment 6 days, to it is above-mentioned after fermentation, taking-up tunning, use deionized water
It is put into baking oven after rinsing 4 times, dry 1.5h, obtains modified expanded perlite at 107 DEG C；The gelatin for being 40% by mass fraction
Solution and spare filtrate and above-mentioned modified expanded perlite are 5 in mass ratio:5:1 is mixed to get mixed liquor, is with concentration
The oxalic acid solution of 1mol/L adjusts pH of mixed to 4, adjusts mixing with the ammonium hydroxide that volume fraction is 1% again after standing reaction 1.5h
Liquid pH to 6, the reaction was continued 25min；Reaction product is poured into surface plate after reaction to above-mentioned, is stood at normal temperature old
Change 47h, obtains plural gel, be in mass ratio 1 by plural gel and deionized water:9h is stood after 5 mixing, is used after standing
Vacuum freeze-drying machine freeze-drying, up to inorganic wall heat-insulating material after discharging.
Example 3
It weighs perlite to be put into high temperature furnace, is heated to 1300 DEG C, calcine 2h, expanded perlite is obtained, by expanded pearlite
The sodium hydroxide solution that rock and mass fraction are 30% is 1 in mass ratio:It is put into autoclave after 5 mixing, sealing reaction
Kettle is heated to 160 DEG C under conditions of pressure is 1.8MPa, high-temperature high-voltage reaction 30min；To it is above-mentioned after reaction,
Filtering, respectively obtains filter residue and filtrate, and filtrate is spare, by filter residue with deionized water repeated flushing 5 times, then by the filter residue after flushing
Mixture is obtained after mixing with castor oil by equal mass ratioes, and mixture is put into fermentor；It is first that above-mentioned fermentor is open
It is placed in the process chamber that temperature is 35 DEG C, relative air humidity is 80%, stands rancid processing 7 days, rancid after treatment is close
Seal fermentation tank mouth, temperature be 40 DEG C at be left to ferment 7 days, to it is above-mentioned after fermentation, taking-up tunning, use deionized water
It is put into baking oven after rinsing 5 times, dry 2h, obtains modified expanded perlite at 110 DEG C；The gelatin for being 40% by mass fraction is molten
Liquid and spare filtrate and above-mentioned modified expanded perlite are 5 in mass ratio:5:1 is mixed to get mixed liquor, is with concentration
The oxalic acid solution of 1mol/L adjusts pH of mixed to 5, adjusts mixed liquor with the ammonium hydroxide that volume fraction is 1% again after standing reaction 2h
PH to 7, the reaction was continued 30min；Reaction product is poured into surface plate after reaction to above-mentioned, it is still aging at normal temperature
48h obtains plural gel, is in mass ratio 1 by plural gel and deionized water:10h is stood after 5 mixing, is used after standing
Vacuum freeze-drying machine freeze-drying, up to inorganic wall heat-insulating material after discharging.
Comparative example
With the inorganic wall heat-insulating material of Hebei company production as a comparison case to inorganic wall heat-insulating material produced by the present invention
Inorganic wall heat-insulating material in material and comparative example carries out performance detection, and testing result is as shown in table 1：
Test method：
Determination of conductive coefficients is tested by national standard GB/T10294-2008.
Water absorption rate test is tested by national standard GB/T 8810-2005.
Tensile strength test is tested by national standard GB/T9641-88, using INSTRON-3300 type universal material testing
Machine is tested for the property.
Intensity test is detected using intensity test machine.
1 wall heat insulation material performance measurement result of table
Low according to the inorganic wall heat-insulating material thermal conductivity produced by the present invention of data among the above, heat insulation effect is good, water suction
Rate is low, will not crack because water suction generates expansion, and tensile strength is high, and compression strength is high, when it receives extraneous stress effect,
Will not swelling cracking, have broad application prospects.
Claims (6)
1. a kind of preparation method of inorganic wall heat-insulating material, it is characterised in that specifically preparation step is：
（1）It weighs perlite to be put into high temperature furnace, calcines, obtain expanded perlite, be 30% by expanded perlite and mass fraction
Sodium hydroxide solution mixing after be put into autoclave, seal reaction kettle, high-temperature high-voltage reaction；
（2）To it is above-mentioned after reaction, filtering, respectively obtain filter residue and filtrate, filtrate is spare, repeatedly with deionized water by filter residue
Rinse 3~5 times, then by after flushing filter residue and castor oil mix after obtain mixture, and mixture is put into fermentor；
（3）First above-mentioned fermentor opening is put in the process chamber, stands rancid processing 5~7 days, rancid after treatment, sealing
Fermentation tank mouth, standing for fermentation take out tunning after fermentation to above-mentioned, are put into baking after being rinsed 3~5 times with deionized water
Case, dry 1~2h, obtains modified expanded perlite at 105~110 DEG C；
（4）By mass fraction be 40% gelatin solution and spare filtrate and above-mentioned modified expanded perlite be mixed to get it is mixed
Liquid is closed, pH of mixed is adjusted to 3~5 with the oxalic acid solution that concentration is 1mol/L, is with volume fraction again after standing 1~2h of reaction
1% ammonium hydroxide adjusts pH of mixed to 6~7, the reaction was continued 20~30min；
（5）Reaction product is poured into surface plate after reaction to above-mentioned, still aging 46~48h, is answered at normal temperature
Gel is closed, 8~10h is stood after plural gel and deionized water are mixed, is freeze-dried after standing with vacuum freeze-drying machine, out
Up to inorganic wall heat-insulating material after material.
2. a kind of preparation method of inorganic wall heat-insulating material according to claim 1, it is characterised in that：Step（1）In
The temperature of the calcining is 1000~1300 DEG C, and the time of calcining is 1~2h, and expanded perlite and mass fraction are 30%
The mass ratio of sodium hydroxide solution is 1:5, the pressure of high temperature and pressure is 1.5~1.8MPa, and the temperature of high-temperature high-voltage reaction is 150
~160 DEG C, 20~30min of time of high-temperature high-voltage reaction.
3. a kind of preparation method of inorganic wall heat-insulating material according to claim 1, it is characterised in that：Step（2）In
The mass ratio of the filter residue and castor oil is 1:1.
4. a kind of preparation method of inorganic wall heat-insulating material according to claim 1, it is characterised in that：Step（3）In
Temperature in the process chamber is 25~35 DEG C, relative air humidity is 65~80%, and the temperature of standing for fermentation is 38~40
DEG C, the time of standing for fermentation is 5~7 days.
5. a kind of preparation method of inorganic wall heat-insulating material according to claim 1, it is characterised in that：Step（4）In
The mass ratio of the gelatin solution and filtrate and modified expanded perlite is 5:5:1.
6. a kind of preparation method of inorganic wall heat-insulating material according to claim 1, it is characterised in that：Step（5）In
The mass ratio of the plural gel and deionized water is 1:5.
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