CN107089810B - A kind of aeroge modified expanded perlite insulation board and preparation method thereof - Google Patents

A kind of aeroge modified expanded perlite insulation board and preparation method thereof Download PDF

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CN107089810B
CN107089810B CN201710277693.2A CN201710277693A CN107089810B CN 107089810 B CN107089810 B CN 107089810B CN 201710277693 A CN201710277693 A CN 201710277693A CN 107089810 B CN107089810 B CN 107089810B
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aeroge
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CN107089810A (en
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郑善
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Tianjin Long Hua Technology Development Co., Ltd.
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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
    • 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
    • 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
    • C04B14/00Use 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
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/04Silica-rich materials; Silicates
    • C04B14/14Minerals of vulcanic origin
    • C04B14/18Perlite
    • C04B14/185Perlite expanded
    • 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
    • C04B16/00Use of organic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of organic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B16/02Cellulosic materials
    • 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
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32Mortars, 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
    • 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
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Abstract

The invention belongs to energy conservation and environmental protection field of material technology, more particularly to it is a kind of building and industrial energy saving heat preservation aeroge modified expanded perlite insulation board, including one or both of swelling perlite powder, aeroge intermediate, cement, batch mixing A, water, ceramic fiber cotton and wood fibre cotton, preparation method is:By one or both of swelling perlite powder, aeroge intermediate, cement, ceramic fiber cotton and wood fibre cotton, it is uniformly mixed, water is added to stir evenly, batch mixing A is added, after stirring evenly, using mold compression moulding, dried after drying to being completely dried.The present invention greatly reduces the thermal coefficient and moisture content of expanded perlite thermal-nsulation panel products, and bending resistance, tensile strength have obtained significantly being promoted.

Description

A kind of aeroge modified expanded perlite insulation board and preparation method thereof
Technical field
The invention belongs to energy conservation and environmental protection field of material technology more particularly to a kind of building and the gas of industrial energy saving heat preservation Gel modified expanded perlite insulation board and preparation method thereof.
Background technology
With the high speed development of social economy, the problem of having become world wide increasingly in short supply of global energy, improves Existing energy utilization rate and the energy saving great attention for having caused various countries.China is the barren country of an energy, because This, reasonable energy utilization, the energy saving sustainable development to Chinese society have great importance.It employs new technology, new work The high efficiency heat insulation material of skill development environment friendly is energy saving most effective most economical one of measure.
In architecture exterior wall insulating materials, used organic insulation material includes polystyrene block, extrusion molding for the country at present Styrofoam, polyurethane foam etc..Organic insulation material heat-insulating property is superior, but fire line is poor, and fire is caused to take place frequently, and this Intensity reduces rapidly after class thermal insulation material is heated in a fire, easy to fall off, causes unnecessary loss.And inorganic heat insulation material is anti- Fiery grade can reach A1 grades, itself non-ignitable, not smoke and thermal stability is good, will not lose intensity because of high temperature.Cause And from energy saving and guarantee life and property safety of people angle, inorganic heat insulation material for building is ground in reinforcement It is imperative to study carefully.
The fire resisting of inorganic external wall thermal-insulation material, environmental protection, intensity is high, long lifespan, but often poor toughness, be easy to happen stress cutting It splits, thermal coefficient is high, causes insulating layer blocked up, is badly in need of solution.
As one kind of inorganic heat insulation material, expanded perlite is with its lightweight (150~250kg/m of bulk density3), compared with Low thermal coefficient (0.058~0.072W/mK), chemical stability good (pH=7), tolerable temperature range wide (200~800 DEG C), non-ignitable (A grades of fire-protection rating), pollution-free, environmentally friendly, long lifespan the features such as paid close attention to by building exterior wall heat preserving industry.So And if the thermal coefficient of the material can be further decreased, the water absorption rate of material is reduced, its toughness and intensity are enhanced, it will be into one Step pushes application of the inorganic heat insulation material in terms of building heat preservation.
The Chinese patent of Patent No. 201510198543.3 discloses a kind of expansible pearlite heat-insulation plate and its system Preparation Method, this method is handled by waterproofing agent of organosilicon reduces the water absorption rate of plank, volume water absorption rate can drop to 5% with Under, but the thermal coefficient of thermal insulation board prepared by the method, in (m DEG C) Zuo You of 0.07W/, thermal coefficient is bigger than normal, heat-insulating property and Toughness is to be improved with intensity.
The Chinese patent of Patent No. 201310577279.5 discloses expanded perlite wall thermal insulation board and its preparation Method, using vitreous expanded perlite, inorganic bonding agent, suitable quantity of water as raw material, prepared heat preservation plate material has preferably the technology Heat insulation effect, and the water resistance of material and mechanical strength do not improve significantly.
Invention content
In view of the technical drawbacks of the prior art, it is an object of the present invention to provide one kind can reduce it is for building swollen The thermal coefficient of swollen pearlite heat-insulation plate improves the aeroge modified expanded perlite insulation board and its system of bending resistance and tensile strength Preparation Method.
The technical solution adopted in the present invention is:
A kind of aeroge modified expanded perlite insulation board includes the expansion of 30~80 parts by weight in parts by weight Crushed crude pearlite, 2~20 parts by weight aeroge intermediates, the batch mixing A of 10~40 parts by weight, the cement of 2~20 parts by weight, 10~ One or both of water A, ceramic fiber cotton and wood fibre cotton of 40 parts by weight;
The batch mixing A in parts by weight, includes the organosilicon of the Ludox of 20~70 parts by weight, 10~50 parts by weight Modified acrylic acid emulsion, the water B of 70~130 parts by weight, the polyacrylamide of 0.05~1 parts by weight, the coupling of 0.5~10 parts by weight Agent A;
The ceramic fiber cotton and the sum of parts by weight of wood fibre cotton addition are swelling perlite powder, among aeroge The 0%~15% of the sum of body, cement weight number.
Preferably, the more excellent parts by weight of the ceramic fiber cotton addition are swelling perlite powder, aeroge intermediate, water The 0.1%~5% of the sum of mud parts by weight;The more excellent parts by weight of the wood fibre cotton addition are swelling perlite powder, gas The 0.5%~10% of the sum of gel intermediate, cement weight number.
Preferably, glass microballoon is also added in thermal insulation board raw material, the parts by weight of the glass microballoon addition are swollen The 0.5%~12% of the sum of swollen crushed crude pearlite, aeroge intermediate, cement weight number.
Preferably, the ceramic fiber cotton, wood fibre cotton length be 1~3mm;The grain size of the swelling perlite powder ≤ 3mm, expansion multiple K0 >=20, density≤1g/cm3
Preferably, water content≤70% of the Ludox, the solid content of the organosilicon-modified acrylic emulsion >= 60%;Ludox is the dispersion liquid of nano level silica dioxide granule in water, the solid content of organosilicon-modified acrylic emulsion Finger lotion in organosilicon-modified acrylic solid content content.
Specifically, the preparation method of the aeroge intermediate, includes the following steps:
(1) mixed solution of silicon source and solvent is prepared
The sodium metasilicate of modulus number 3.0~4.0 is fitted into reaction kettle, and the water C progress that 1~3 times of sodium metasilicate quality is added is dilute It releases, reaction kettle obtains sodium silicate solution with the speed stirring 30min of 80~200r/min through 200 mesh screens;
The aqueous solution of sodium metasilicate is commonly called as waterglass, it is made of the alkali metal and silica of different proportion, changes Formula is R2O·nSiO2, R in formula2O is alkali metal oxide, and n is the ratio of silica and alkali metal oxide molal quantity, The referred to as modulus of waterglass, the most commonly used is sodium silicate water glass Na2O·nSiO2
(2) colloidal sol
It takes A sour, A acid metal salts is added in A acid and rare earth A hydrochlorates are added in a manner of spray to step after mixing Suddenly the sodium silicate solution that (1) obtains;The material in reaction kettle is carried out soon with the speed of 1200~2000r/min while spray Speed stirring, the pH value for controlling sodium silicate solution is 1.5~3.0, and it is 15~30 nanometers to control its average pore size, obtains colloidal sol, this 60~120min of step used time;
Preferably, the A acid is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, and 6~15mol/L is adjusted to water E;
Preferably, the A acid metal salts are A acid zirconates or A acid aluminium salts;
Preferably, the rare earth A hydrochlorates are A acid cerium salt, A acid yttrium salt or A acid lanthanum salts;
A acid metal salts and rare earth A hydrochlorates are easy the moisture absorption, and metering can be caused inaccurate, so for its addition of accurate quantitative analysis Amount, in terms of oxide, the molar ratio of the two is 100 for A acid metal salts described in above-mentioned steps (2) and rare earth A hydrochlorates:1~6;Step Suddenly in (2) in the oxide and sodium metasilicate of A acid metal salts silica molar ratio 2~5:100;For example, A acid metal salts are sulfuric acid Aluminium, in terms of its oxide, i.e., with the molar ratio of silica in aluminium oxide and sodium metasilicate for 2~5:100;
(3) gel
Sodium hydroxide or ammonium hydroxide are taken, it is 10~11.5 that water D, which is added, and is diluted to pH value, is added in a manner of spray to reaction kettle In;The material in reaction kettle is quickly stirred with the speed of 1200~2000r/min while spray, when object in reaction kettle When the pH value of material is 4.5~5.5, spray is terminated, gel, 80~180min of this step used time are obtained;
(4) aging
3~10h of stirring is continued with the speed of 20~50r/min in reaction kettle, aging, control are carried out to the material in reaction kettle Material in reactor temperature processed is 35~50 DEG C;The mode that standing is usually used in the prior art carries out aging, takes 3~5 days, Gel can't be stirred, the reason is that the prior art needs to stand during generally believing aging, standing can Convenient for the structure growth of aeroge;
(5) solvent is replaced
It carries out continuing 60~180min of stirring in reaction kettle, while being added same with aging material in step (4) reaction kettle The displacement solvent of volume, to displace remaining moisture;The prior art worries that stirring can destroy its structure, will not generally replace When be stirred, stewing process can be taken, cause take it is longer;Preparation method provided by the invention is stirred when solvent is replaced 60~180min is mixed, can greatly shorten period of a permutation, there is no destroyed microstructure;
Preferably, the displacement solvent is one or more of mixtures of methanol, acetone, n-hexane or heptane;
(6) surface modification
It carries out continuing stirring in reaction kettle, while continuously adding and aging material same volume in step (4) reaction kettle Coupling agent B;By stirring 60~180min, obtain being coated among the rare earth toughening silica aerogel of displacement solvent and coupling agent B Body, the aeroge intermediate as added in raw material;
The coupling agent B that above-mentioned steps (6) surface modification is added cements out the water in aeroge micropore, and coupling agent B is filled out It is charged into aeroge micropore, the stability of microcellular structure can be improved, improve the evenness of pore size;In addition, by pair plus Enter after different coupling agent B is surface modified, aeroge hydrophobicity, hydrophilic sexual function can be adjusted;
Preferably, coupling agent B described in above-mentioned steps (6) be hexamethyldisilazane, bis- (trimethylsilyl) acetamides, Methoxytrimethylsilane, dimethoxydimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyl The one or more of trimethoxy silane, methyltriethoxysilane and methyl trimethoxy oxygroup alkane;
Preferably, the stirring described in above-mentioned steps (5) or step (6) is to be stirred in reaction kettle;
Preferably, the stirring provides for reaction kettle center and quickly forward stirs (high speed shear disk), reaction kettle center Periphery provide baffle plate to realize.
The water A, water B, water C, water D are deionized water.
The above-mentioned aeroge intermediate using normal temperature and pressure technique productions is a kind of light porous amorphous state of structure-controllable There is inorganic nano material continuous tridimensional network, porosity to be up to 80% or more, and average pore size is 20nm or so, than Surface area is more than 500 ㎡/g, and density is less than 70kg/m3, thermal coefficient is less than 0.020W/ (mK) under normal temperature and pressure, than static The thermal conductivity 0.022W/ (mK) of air is also low, be at present rare low cost, industrialization, low heat conductivity solid material.
A kind of preparation method of aeroge modified expanded perlite insulation board, including follow the steps below successively:
(1) primary election of swelling perlite powder:Sizing screening is carried out to expanded perlite, selects the expansion of diameter grain≤3mm precious Pearl rock powder;
(2) separation of swelling perlite powder:Primary election swelling perlite powder is passed through into cyclone separator, selects expansion multiple K0 >=20, density≤1g/cm3Swelling perlite powder, as swelling perlite powder;
(3) preparation of batch mixing A:Take 20~70 parts by weight of Ludox, 10~50 weight of organosilicon-modified acrylic emulsion Part, the parts by weight of water B70~130,0.05~1 parts by weight of polyacrylamide, the parts by weight of coupling agent A0.5~10, stir evenly, and turn Speed is 500~1000r/min, and mixing time is that 30~50min obtains batch mixing A;Batch mixing A is bonding agent;
(4) preparation of total batch mixing:Take the swelling perlite powders of 30~80 parts by weight, 2~20 parts by weight aeroge intermediates, The sum of the cement of 2~20 parts by weight, parts by weight are swelling perlite powder and the sum of aeroge intermediate and cement weight number One or both of 0%~15% ceramic fiber cotton and wood fibre cotton, are mediated using kneader, and kneader rotating speed is 50 ~200r/min, kneading time are 20~50min, and 10~40 parts by weight water A are added, are mediated using kneader, kneader rotating speed For 50~200r/min, kneading time is 20~50min, is eventually adding the batch mixing A of 10~40 parts by weight, stirs evenly, and is stirred 500~1000r/min of rotating speed, mixing time are 30~50min, obtain total batch mixing;
(5) preparation of blank:Using mold by total batch mixing compression moulding, total batch mixing fills and leads up mold, pressure be 0.4~ 1.2kPa, compression ratio control are molded, institute's moulding material is aeroge expanded pearlite at this time under conditions of 1.1~1.8 Rock heat preservation plate material blank;
(6) preparation of product:Above-mentioned blank, blank are placed in 95~105 DEG C of environment, then 5~45min of constant temperature drying dries in the air Shining one week can be completely dried, and obtain aeroge expanded perlite thermal-nsulation plate product;The process of constant temperature drying keeps cement quick Reaction, setting rate is fast, it is made to reach intensity requirement as early as possible.
Preferably, in the step (4), swelling perlite powder, aeroge intermediate, cement, ceramic fiber cotton with it is wooden Before one or both of cellucotton is mediated using kneader, it also added in raw material in swelling perlite powder, aeroge The glass microballoon of the sum of mesosome, cement weight number 0.5%~12%.
Preferably, total batch mixing made from the step (5) carries out foaming processing before compression moulding, and processing procedure is: Physical blowing agent is added in total batch mixing and foaming processing is carried out using foaming machine, the parts by weight that foaming agent is added are cement weight The 0.1%~1.5% of number is measured, kneader is inputted in foaming, kneader rotating speed is 50~200r/min, kneading time 20 ~50min uses mold compression moulding after kneading.
The mixing of all solid materials all stirs material with planetary mixer in the preparation process of thermal insulation board, contains liquids The stirring of material is stirred using kneader.
The present invention operation principle be:
Aeroge is also known as blue smoke, with following characteristic:1, several infinite more nano-pores are distributed in the inside of aeroge And air vent wall, air can not be flowed freely in nanometer stomata, be relatively adsorbed on air vent wall, aerogel material is in class Likelihood dummy status, effectively reduces convection current heat transfer, and heat is transmitted in solid material and can be transmitted along air vent wall;These air vent wall structures At the heat conduction path of infinite length, this will substantially reduce heat conduction;2, there are infinite more gas inside aeroge intermediate Hole wall, air vent wall are equivalent to infinite more thermal baffle, the reflection to light and heat may be implemented, and are passed to which radiation be greatly lowered Heat;3, aeroge can effectively penetrate sunlight, and prevent the infrared emanation of environment temperature, become a kind of ideal septum pellucidum Hot material makes the thermal conductivity of material substantially reduce;
Based on the characteristic of above-mentioned aeroge, suitable bonding agent is selected, by aeroge and industry, building heat preservation thermal insulation board Making material combines, and can not only enhance industrial, building heat preservation thermal insulation board mechanical strength, additionally it is possible to effectively reduce its heat conduction Coefficient, improves its insulation ability, improves hydrophobic rate, improve industry and building heat preservation with heat preservation plate surface and wall or other The binding ability of material.
Compared with traditional handicraft, the beneficial effects of the present invention are:
1, currently, although organic insulation material thermal coefficient is relatively low, since its fire resistance is poor, limit It is applied;Expanded perlite thermal-nsulation plate is inorganic heat insulation material, and the thermal coefficient of best expanded perlite thermal-nsulation plate exists 0.058w/m.k or more, it is always tired how its thermal coefficient to be reduced to 0.043w/m.k or less and can reach the fire prevention of A1 ranks Disturb the technical barrier of those skilled in the art;
Products obtained therefrom of the present invention is inorganic heat insulation material, and aeroge intermediate is added to expanded perlite thermal-nsulation by the present invention In plate, due to the presence of nanometer three-dimensional structure in aeroge intermediate, aeroge expanded perlite thermal-nsulation plank obtained has The incomparable heat-proof quality of traditional material, the thermal coefficient of product can reach 0.035~0.045w/m.k, realize The low thermal conductivity of fire prevention A1 ranks, environment protection architecture thermal insulation material;
2, aeroge is added in the form of powder in existing thermal insulation board, and aerogel powder has to pass through in preparation process It is dried, drying process is to use supercritical drying process to complete at high temperature under high pressure, and working condition is harsh, and technique is multiple Miscellaneous, dangerous big, process units investment is big, and preparation efficiency is low, and raw material are of high cost based on the silanol of high price;
Aeroge in thermal insulation board of the present invention is added in the form of aeroge intermediate, raw without drying process step It produces at low cost;In addition, aeroge intermediate is to prepare at normal temperatures and pressures, stabilization simple for process is safe, technical process from Traditional 300h is down to 30h, and the process units investment of same production capacity is only the 1/20 of conventional method, and the prices of raw materials compare traditional silicon Low 100 times of source or more, product cost are only the 1/10 of conventional method;
3, product moisture content is less than 0.2% in the present invention, and water absorbing properties significantly reduce, and water resistance significantly improves;
4, the aeroge expanded perlite thermal-nsulation plank in the present invention increases building simultaneously in thinned thermal insulation material thickness Usable floor area, it is highly beneficial to expanding the small apartment interior space;
5, product maintains the advantages such as inexpensive, nuisanceless, low unit weight, A1 grades of fire prevention, long lifespan, environmental protection in the present invention;
6, after expanded perlite being added in plank raw material, the thermal coefficient of expanded perlite is considerably reduced;
7, the wood fibre cotton used in the present invention plays the role of enhancing heat insulation and heat preservation, pottery for porous material Porcelain cellucotton plays the role of integrally stretching;
8, of the invention to prepare glass microballoon in raw material and selectively add, since glass microballoon is porous material, add The heat insulation of thermal insulation board can be further enhanced after adding glass microballoon, production can be saved if preparing and omitting glass microballoon in raw material Cost;
9, batch mixing A is bonding agent, and since the addition of bonding agent substantially increases the toughness of the heat preservation plate material, flexural strength can To reach 0.36Mpa, tensile strength is more than 0.1Mpa, eliminates the material caused by construction material coefficient of expansion difference Stress cracking;
10, wet concentration deionized water in the present invention, the low cost of deionized water are conducive to further decrease production cost;
11, product is cement base in the present invention, and expanded perlite needs to be bonded together by cement, if using water merely Mud bonds, and thermal coefficient is higher;Novelty of the present invention introduces the mode of physical blowing, and micron level is added in cement Stomata keeps cement composition loose, nano level stomata is contained in aeroge, expanded perlite, glass microballoon, wood fibre cotton are equal To include leachy porous material, a kind of various sizes of mode of grading of stomatal limiting value further enhances the heat-insulated of product Effect;
12, traditional cement foamed mode foams for chemical method, and one is generate two using aluminium powder and alkali for chemical blowing Carbonoxide foams, and another kind is to use dioxygen Water blown, but the mode of chemical blowing must have corresponding environment and temperature, no It is suitble to large batch of commercial application;Cement in the present invention carries out physical blowing using physical blowing agent, to environment and temperature It is required that not stringent, the bubble sent out is very thin and has certain viscosity, not fragile, can directly add in plate and use, and is suitble to large quantities of The commercial application of amount;
13, total batch mixing is molded by foaming processing is re-compacted compared with the not foamed processing direct pressing molding of total batch mixing, Its thermal coefficient declines 0.005w/m.k;
14, in the preparation process of thermal insulation board, the stirring of material is all made of conventional concrete blender, and paddle is in spiral shell Shape is revolved, the non-uniform phenomenon of material stirring is susceptible to;Solid material stirs material, rotating speed using planetary mixer in the present invention Fast and Multi-angle turnover material avoids cement too big with other material ratio heavy phase differences and lamination occurs, material mixing Highly uniform, the product quality produced is uniform, and the performances performance such as heat preservation, anti-folding, bending resistance is more preferably;
15, the compression ratio of traditional thermal insulation board is controlled 1.2;The present invention controls compression ratio 1.3~1.6, passes through control Compression ratio processed effectively controls panel density, ensures that plank has good mechanical strength, compressive property, bending strength, tension strong Degree;
16, the operation principle that in the present invention prepared by aeroge intermediate is:In the preparation method of aeroge intermediate, gel The A acid metal salts and rare earth A hydrochlorates being added in the process can achieve the effect that toughening and improve silica aerogel heat resistance;Aging It is to carry out in the state of stirring with solvent swap step, substantially increases reaction efficiency, have compressed the process time, is suitble to production Industry;
17, compared with prior art, advantage has the following to preparation among aeroge in the present invention:
(1) in recent years, there are some about relevant report and the patent text for preparing aeroge under room temperature differential pressure in the prior art It offers, but is to rest on laboratory preparatory phase mostly, technical process is longer, while process implementing narrow limits, it is difficult to realize Large-scale industrialized production and application;The present invention provides the preparation methods under normal temperature and pressure, and it is opposing stationary to change the prior art Technique, apply in critical process process and stir, speeded up to the hydrolysis, polycondensation and modification of aeroge, realize in 30h and close At the technique of aeroge intermediate, a kind of method that industrial batch prepares rare earth toughening aeroge is provided, is aeroge A large amount of manufacture and use provide premise;
(2) one of hinder the reason of aeroge development that be aeroge have reticular structure, but the structure in the prior art Edge it is relatively thin, more crisp, compression strength is low, and easy compression is caved in, and causes performance unstable;Present invention addition rare earth A hydrochlorates With A acid metal salts, the toughness of the material is improved, improves the intensity of aeroge;
(3) temperature in use of the aeroge of prior art preparation is relatively low, generally used below also more stable at 500 DEG C, 500 DEG C or more the internal structure changes that can lead to aeroge, cause thermal coefficient to decline;The present invention addition rare earth A hydrochlorates and A Acid metal salt improves the heat resistance of the material, improves the heat resisting temperature of aeroge.
18, the three-dimensional structure of aeroge plays an important role during its performance plays, if in aeroge Hole be combined agent and block and can not just play a role;
Traditional aeroge is prepared at high temperature under high pressure, if the later stage is not specially treated, porous three-dimensional space It is easy to be combined agent or other raw materials is blocked and failed, and then it is made to lose heat insulation, in addition, aeroge is porous three-dimensional vertical Body spaces union can play better thermal insulation together, can found the three-dimensional inside aeroge after being separated by binder Isolated island is isolated into body space, and then generates island effect, reduces the heat insulation of aeroge;
It is occupied in aeroge containing displacement solvent, displacement solvent in the aeroge intermediate prepared using method in the present invention Between porous three-dimensional space in vivo, bonding agent or other raw materials can not invade it is porous in occupy its three-dimensional space, protect In warm plate drying process, displacement solvent volatilization is maintained to porous 3 D stereo after solvent volatilizees in aeroge Structure overcomes failure and island effect caused by hole is blocked, and therefore, heat-proof quality is stronger.
In short, compared with conventional expanded pearlite insulation panel products, the present invention greatly reduces expanded perlite thermal-nsulation The thermal coefficient and water absorption rate of panel products, bending resistance, tensile strength have obtained significantly being promoted, and maintain low cost, A1 The advantages such as grade fire prevention, are building energy conservation, environmental protection, provide a kind of new material.
Specific implementation mode
With reference to embodiment, the invention will be further described:
One, Examples 1 to 8
1, a kind of formula of aeroge modified expanded perlite insulation board, in parts by weight, including 30~80 weight The swelling perlite powder of part, the water of 2~20 parts by weight aeroge intermediates, the batch mixing A of 10~40 parts by weight, 2~20 parts by weight One or both of mud, the water A of 10~40 parts by weight, ceramic fiber cotton and wood fibre cotton, each raw material in Examples 1 to 8 Specific dosage referring to table 1;
In parts by weight, including the Ludox of 20~70 parts by weight, 10~50 parts by weight is organic-silicon-modified by batch mixing A Acrylic emulsion, the water B of 70~130 parts by weight, the polyacrylamide of 0.05~1 parts by weight, 0.5~10 parts by weight coupling agent A, the component detail of batch mixing A is referring to table 2 in Examples 1 to 8;
The sum of parts by weight of ceramic fiber cotton and wood fibre cotton addition are swelling perlite powder, aeroge intermediate, The 0%~15% of the sum of cement weight number;
In thermal insulation board raw material also be added with glass microballoon, glass microballoon addition parts by weight be swelling perlite powder, The 0.5%~12% of the sum of aeroge intermediate, cement weight number;
Wherein, ceramic fiber cotton, wood fibre cotton length be 1~3mm;Grain size≤3mm of swelling perlite powder, it is swollen Swollen multiple K0 >=20, density≤1g/cm3;Water content≤70% of Ludox, the solid content of organosilicon-modified acrylic emulsion >= 60%, water A, water B are deionized water.
The raw material detail list of aeroge modified expanded perlite insulation board in 1 Examples 1 to 8 of table
Batch mixing component A is detailed in 2 Examples 1 to 8 of table
2, a kind of preparation method of aeroge modified expanded perlite insulation board, prepares, in accordance with the following steps in each step The concrete numerical value of parameter is referring to table 3:
(1) primary election of swelling perlite powder:Sizing screening is carried out to expanded perlite, selects the expansion of diameter grain≤3mm precious Pearl rock powder;
(2) separation of swelling perlite powder:Primary election swelling perlite powder is passed through into cyclone separator, selects expansion multiple K0 >=20, density≤1g/cm3Swelling perlite powder, as swelling perlite powder;
(3) preparation of batch mixing A:Take 20~70 parts by weight of Ludox, 10~50 weight of organosilicon-modified acrylic emulsion Part, the parts by weight of water B70~130,0.05~1 parts by weight of polyacrylamide, the parts by weight of coupling agent A0.5~10, stir evenly, stir Mix rotating speed is 500~1000r/min, and mixing time is 30~50min, obtains batch mixing A;
(4) preparation of total batch mixing:Take the swelling perlite powders of 30~80 parts by weight, 2~20 parts by weight aeroge intermediates, The sum of the cement of 2~20 parts by weight, parts by weight are swelling perlite powder and the sum of aeroge intermediate and cement weight number One or both of 0%~15% ceramic fiber cotton and wood fibre cotton, selectivity add swelling perlite powder, aeroge The glass microballoon of the sum of intermediate, cement weight number 0.5%~12% is mediated for the first time using kneader, and kneader turns Speed is 50~200r/min, and kneading time is 20~50min, and the water A of 10~40 parts by weight is added, and is carried out using kneader secondary It mediates, kneader rotating speed is 50~200 r/min, and kneading time is 20~50min, is eventually adding the batch mixing of 10~40 parts by weight A is stirred evenly, 500~1000r/min of speed of agitator, and mixing time is 30~50min, obtains total batch mixing;
(5) foaming is handled:Physical blowing agent is added in total batch mixing and foaming processing is carried out using foaming machine, foaming agent adds The parts by weight entered are the 0.1%~1.5% of cement weight number, and kneader input in foaming, kneader rotating speed for 50~ 200r/min, kneading time are 20~50min, and mold compression moulding is used after kneading;
(6) preparation of blank:Using mold by total batch mixing compression moulding, total batch mixing fills and leads up mold, pressure be 0.4~ 1.2kPa, compression ratio control are molded, institute's moulding material is aeroge expanded pearlite at this time under conditions of 1.1~1.8 Rock heat preservation plate material blank;
(7) preparation of product:Above-mentioned blank is placed in 95~105 DEG C of environment, then 5~45min of constant temperature drying is dried one week It can be completely dried, obtain aeroge expanded perlite thermal-nsulation plate product.
The mixing of all solid materials all stirs material with planetary mixer in the preparation process of thermal insulation board, contains liquids The stirring of material is stirred using kneader.
The specific number of parameter in each step of preparation method of 3 Examples 1 to 8 aeroge modified expanded perlite insulation board of table Value
3, the specific preparation process of the aeroge intermediate used in aeroge modified expanded perlite insulation board is as follows:
(1) mixed solution of silicon source and solvent is prepared
The waterglass of modulus number 3.0~4.0 is fitted into reaction kettle, and the water C progress that 1~3 times of waterglass quality is added is dilute It releases, reaction kettle obtains water glass solution with the speed stirring 30min of 80~200r/min through 200 mesh screens;
(2) colloidal sol
It takes A sour, A acid metal salts is added in A acid and rare earth A hydrochlorates are added in a manner of spray to step after mixing Suddenly the water glass solution that (1) obtains;The material in reaction kettle is carried out soon with the speed of 1200~2000r/min while spray Speed stirring, control ph to 1.5~3.0 stop spray, and spray time is controlled in 60~120min, obtains colloidal sol;
A acid is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, its concentration is adjusted to 6~15mol/L with water E;
A acid metal salts are A acid zirconates or A acid aluminium salts, and rare earth A hydrochlorates are A acid cerium salt, A acid yttrium salt or A acid lanthanum salts;
In terms of oxide, the molar ratio of the two is 100 for A acid metal salts and rare earth A hydrochlorates:1~6;
The molar ratio 2~5 of silica in the oxide and water glass solution of A acid metal salts:100;
(3) gel
Sodium hydroxide or ammonium hydroxide are taken, it is 10~11.5 that water D, which is added, and is diluted to pH value, is added in a manner of spray to step (2) in reaction kettle in gained colloidal sol;The material in reaction kettle is carried out soon with the speed of 1200~2000r/min while spray Speed stirring sprays 80~180min of used time, obtains gel when the pH value of material in reactor is 4.5~5.5;
(4) aging
3~10h of stirring is continued with the speed of 20~50r/min in reaction kettle, aging, control are carried out to the material in reaction kettle Material in reactor temperature processed is 35~50 DEG C;
(5) solvent is replaced
The displacement solvent with aging material same volume in step (4) reaction kettle is added while stirring in reaction kettle, with Remaining moisture is displaced, 60~180min is stirred;
Displacement solvent is one or more of mixtures of methanol, acetone, n-hexane or heptane;
(6) surface modification
It carries out continuing stirring in reaction kettle, while continuously adding and aging material same volume in step (4) reaction kettle Coupling agent B obtains the rare earth toughening silicon for being coated with displacement solvent and coupling agent B after surface modification by stirring 60~180min Aeroge intermediate, the aeroge intermediate as added in raw material;
Stirring in step (5) or step (6) is that heart offer is quickly forward stirred in a kettle, reaction kettle center Periphery provides baffle plate;
Coupling agent is hexamethyldisilazane, bis- (trimethylsilyl) acetamides, methoxytrimethylsilane, dimethoxy two Methyl-monosilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyltrimethoxysilane, methyltriethoxy silane One or more of mixtures of alkane and methyl trimethoxy oxygroup alkane;Water C, water D, water E are deionized water.
The variable parameter of each embodiment and concrete numerical value are shown in Table 4 in the preparation method of aeroge intermediate.
The design parameter that step (1)~(6) use in the preparation method of aeroge intermediate in 4 Examples 1 to 8 of table
Embodiment 9~16
The contrast groups embodiment 9~16 of Examples 1 to 8 is respectively set, embodiment 9~16 is in the preparation process of thermal insulation board Not foamed processing procedure;Rest part, embodiment 9 is with embodiment 1, and embodiment 10 is the same as embodiment 2,11 same embodiment of embodiment 3, embodiment 12 is with embodiment 4, and embodiment 13 is with embodiment 5, and for embodiment 14 with embodiment 6, embodiment 15 is real with embodiment 7 Example 16 is applied with embodiment 8;
In embodiment 9~16, the preparation method of aeroge modified expanded perlite insulation board carries out in accordance with the following steps, The concrete numerical value of parameter is referring to table 5 in each step:
(1) primary election of swelling perlite powder:Sizing screening is carried out to expanded perlite, selects the expansion of diameter grain≤3mm precious Pearl rock powder;
(2) separation of swelling perlite powder:Primary election swelling perlite powder is passed through into cyclone separator, selects expansion multiple K0 >=20, density≤1g/cm3Swelling perlite powder, as swelling perlite powder;
(3) preparation of batch mixing A:Take 20~70 parts by weight of Ludox, 10~50 weight of organosilicon-modified acrylic emulsion Part, the parts by weight of water B70~130,0.05~1 parts by weight of polyacrylamide, the parts by weight of coupling agent A0.5~10, stir evenly, stir Mix rotating speed is 500~1000r/min, and mixing time is 30~50min, obtains batch mixing A;
(4) preparation of total batch mixing:Take the swelling perlite powders of 30~80 parts by weight, 2~20 parts by weight aeroge intermediates, The sum of the cement of 2~20 parts by weight, parts by weight are swelling perlite powder and the sum of aeroge intermediate and cement weight number One or both of 0%~15% ceramic fiber cotton and wood fibre cotton, selectivity add swelling perlite powder, aeroge The glass microballoon of the sum of intermediate, cement weight number 0.5%~12% is mediated for the first time using kneader, and kneader turns Speed is 50~200r/min, and kneading time is 20~50min, and the water A of 10~40 parts by weight is added, and is carried out using kneader secondary It mediates, kneader rotating speed is 50~200 r/min, and kneading time is 20~50min, is eventually adding the batch mixing of 10~40 parts by weight A is stirred evenly, 500~1000r/min of speed of agitator, and mixing time is 30~50min, obtains total batch mixing;
(5) preparation of blank:Using mold by total batch mixing compression moulding, total batch mixing fills and leads up mold, pressure be 0.4~ 1.2kPa, compression ratio control are molded, institute's moulding material is aeroge expanded pearlite at this time under conditions of 1.1~1.8 Rock heat preservation plate material blank;
(6) preparation of product:Above-mentioned blank is placed in 95~105 DEG C of environment, then 5~45min of constant temperature drying is dried one week It can be completely dried, obtain aeroge expanded perlite thermal-nsulation plate product.
The mixing of all solid materials all stirs material with planetary mixer in the preparation process of thermal insulation board, contains liquids The stirring of material is stirred using kneader.
Parameter is specific in each step of preparation method of 5 embodiment of table, 9~16 aeroge modified expanded perlite insulation board Numerical value
Two, performance detection
Product of the present invention is plate-like, is detected to the product in embodiment 1~16.
(1) according to method specified in GB/T 10294 in embodiment 1~16 heat preservation panel products thermal coefficient into Row detection;
(2) tensile strength of the heat preservation panel products in embodiment 1~16 is examined according to method specified in JGJ 144 It surveys;
(3) according to method specified in GB/T 11969 in embodiment 1~16 heat preservation panel products flexural strength into Row detection;
(4) water resistance detects:According to method specified in GB/T 11969 to the heat preservation panel products in embodiment 1~16 Moisture content be detected;
(5) combustibility of the heat preservation panel products in embodiment 1~16 is examined according to method specified in GB 8624 It surveys;
Specific testing result is shown in Table 6, table 7.
The testing result of product in 6 Examples 1 to 8 of table
The testing result of product in 7 embodiment 9~16 of table
By table 6, table 7 it is found that the thermal coefficient of product of the present invention can reach 0.035~0.045w/m.k, at other In the case of part all same, for total batch mixing after foaming is handled, the thermal coefficient of final products reduces 0.005w/m.k;This hair The flexural strength of bright product can reach 0.36Mpa, and tensile strength is more than 0.1Mpa and realizes A1 grades of fire prevention;In the present invention Product moisture content is less than 0.2%, and water absorbing properties significantly reduce, and water resistance significantly improves.
The application method of product is identical as the application method of conventional vacuum plate in the present invention.
16 embodiments of the present invention are described in detail above, but the content is only the preferable implementation of the present invention Example should not be construed as limiting the practical range of the present invention.It is all according to all the changes and improvements made by the present patent application range Deng should all still fall within the scope of the patent of the present invention.

Claims (9)

1. a kind of aeroge modified expanded perlite insulation board, it is characterised in that:In parts by weight, including 30~80 weight The swelling perlite powder of part, the water of 2~20 parts by weight aeroge intermediates, the batch mixing A of 10~40 parts by weight, 2~20 parts by weight One or both of mud, the water A of 10~40 parts by weight, ceramic fiber cotton and wood fibre cotton;
In parts by weight, including the Ludox of 20~70 parts by weight, 10~50 parts by weight is organic-silicon-modified by the batch mixing A Acrylic emulsion, the water B of 70~130 parts by weight, the polyacrylamide of 0.05~1 parts by weight, 0.5~10 parts by weight coupling agent A;
The sum of parts by weight of the ceramic fiber cotton and wood fibre cotton addition are swelling perlite powder, aeroge intermediate, The 0%~15% of the sum of cement weight number;
The preparation method of the aeroge intermediate, includes the following steps:
(1) mixed solution of silicon source and solvent is prepared
The sodium metasilicate of modulus number 3.0~4.0 is fitted into reaction kettle, and the water C that 1~3 times of sodium metasilicate quality is added is diluted, and is reacted Kettle obtains sodium silicate solution with the speed stirring 30min of 80~200r/min through 200 mesh screens;
(2) colloidal sol
It takes A sour, A acid metal salts is added in A acid and rare earth A hydrochlorates are added in a manner of spray to step after mixing (1) sodium silicate solution obtained;The material in reaction kettle is carried out quickly with the speed of 1200~2000r/min while spray Stirring, the pH value for controlling sodium silicate solution is 1.5~3.0, obtains colloidal sol;
The A acid is sulfuric acid, hydrochloric acid, oxalic acid or nitric acid, and 6~15mol/L is adjusted to water E;
The A acid metal salts are A acid zirconates or A acid aluminium salts;
The rare earth A hydrochlorates are A acid cerium salt, A acid yttrium salt or A acid lanthanum salts;
(3) gel
Sodium hydroxide or ammonium hydroxide are taken, it is 10~11.5 that water D, which is added, and is diluted to pH value, is added into reaction kettle in a manner of spray; The material in reaction kettle is quickly stirred with the speed of 1200~2000r/min while spray, works as material in reactor PH value be 4.5~5.5 when, terminate spray, obtain gel;
(4) aging
3~10h of stirring is continued with the speed of 20~50r/min in reaction kettle, aging is carried out to the material in reaction kettle, control is anti- It is 35~50 degrees Celsius to answer material temperature in kettle;
(5) solvent is replaced
It carries out continuing 60~180min of stirring in reaction kettle, while being added and aging material same volume in step (4) reaction kettle Displacement solvent, to displace remaining moisture;
(6) surface modification
It carries out continuing stirring in reaction kettle, while continuously adding the coupling with aging material same volume in step (4) reaction kettle Agent B;By stirring 60~180min, the aeroge intermediate for being coated with displacement solvent and coupling agent B is obtained;
The coupling agent B is hexamethyldisilazane, bis- (trimethylsilyl) acetamides, methoxytrimethylsilane, dimethoxy Dimethylsilane, phenyl triethoxysilane, phenyltrimethoxysila,e, vinyltrimethoxysilane, methyl triethoxy The one or more of silane and methyl trimethoxy oxygroup alkane.
2. a kind of aeroge modified expanded perlite insulation board according to claim 1, it is characterised in that:The ceramics are fine Vinylon and cotton blend adds 0.1%~5% that parts by weight are the sum of swelling perlite powder, aeroge intermediate, cement weight number;It is described The parts by weight of wood fibre cotton addition be swelling perlite powder, aeroge intermediate, the sum of cement weight number 0.5%~ 10%.
3. a kind of aeroge modified expanded perlite insulation board according to claim 1, it is characterised in that:Thermal insulation board former material Glass microballoon is also added in material, the parts by weight of the glass microballoon addition are swelling perlite powder, aeroge intermediate, water The 0.5%~12% of the sum of mud parts by weight.
4. a kind of aeroge modified expanded perlite insulation board according to claim 1, it is characterised in that:The ceramics are fine Vinylon and cotton blend, wood fibre cotton length be 1~3mm;Grain size≤3mm of the swelling perlite powder, expansion multiple K0 >=20, density ≤1g/cm3
5. a kind of aeroge modified expanded perlite insulation board according to claim 1, it is characterised in that:The Ludox Water content≤70%, solid content >=60% of the organosilicon-modified acrylic emulsion.
6. a kind of aeroge modified expanded perlite insulation board according to claim 1, it is characterised in that:The water A, water B, water C, water D are deionized water.
7. special according to a kind of preparation method of any aeroge modified expanded perlite insulation boards of claim 1-6 Sign is, including follows the steps below successively:
(1) primary election of swelling perlite powder:Sizing screening is carried out to expanded perlite, selects the expanded perlite of diameter grain≤3mm Powder;
(2) separation of swelling perlite powder:The swelling perlite powder of primary election is passed through into cyclone separator, select expansion multiple K0 >= 20, density≤1g/cm3Swelling perlite powder;
(3) preparation of batch mixing A:Take 20~70 parts by weight of Ludox, 10~50 parts by weight of organosilicon-modified acrylic emulsion, water The parts by weight of B70~130,0.05~1 parts by weight of polyacrylamide, the parts by weight of coupling agent A0.5~10, stir evenly, obtain batch mixing A;
(4) preparation of total batch mixing:Take the swelling perlite powders of 30~80 parts by weight, 2~20 parts by weight aeroge intermediates, 2~ The sum of the cement of 20 parts by weight, parts by weight are swelling perlite powder and the sum of aeroge intermediate and cement weight number 0% One or both of~15% ceramic fiber cotton and wood fibre cotton, are mediated using kneader, and 10~40 parts by weight are added Water A, kneader mediate, be eventually adding the batch mixing A of 10~40 parts by weight, stir evenly, obtain total batch mixing;
(5) preparation of blank:Using mold by total batch mixing compression moulding, total batch mixing fills and leads up mold, pressure be 0.4~ 1.2kPa, compression ratio control are molded, institute's moulding material is aeroge expanded pearlite at this time under conditions of 1.1~1.8 Rock heat preservation plate material blank;
(6) preparation of product:Above-mentioned blank is dried after drying to being completely dried, and aeroge expanded perlite thermal-nsulation is obtained Plate product.
8. a kind of preparation method of aeroge modified expanded perlite insulation board according to claim 7, it is characterised in that: In the step (4), swelling perlite powder, aeroge intermediate, cement, ceramic fiber cotton and one kind in wood fibre cotton or Before two kinds are mediated using kneader, swelling perlite powder, aeroge intermediate, cement weight number are also added in raw material The sum of 0.5%~12% glass microballoon.
9. a kind of preparation method of aeroge modified expanded perlite insulation board according to claim 7, it is characterised in that: Total batch mixing made from the step (5) carries out foaming processing before compression moulding, and processing procedure is:The admixture in total batch mixing Haircut infusion simultaneously carries out foaming processing using foaming machine, the parts by weight that foaming agent is added be cement weight number 0.1%~ 1.5%, kneader kneading is inputted in foaming, and mold compression moulding is used after kneading.
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