CN107777979A - A kind of natural halloysite clay aeroge for building heat preservation and preparation method thereof - Google Patents

A kind of natural halloysite clay aeroge for building heat preservation and preparation method thereof Download PDF

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Publication number
CN107777979A
CN107777979A CN201610779233.5A CN201610779233A CN107777979A CN 107777979 A CN107777979 A CN 107777979A CN 201610779233 A CN201610779233 A CN 201610779233A CN 107777979 A CN107777979 A CN 107777979A
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halloysite clay
natural
clay
aeroge
ethyl alcohol
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刘洪丽
何翔
李洪彦
褚鹏
李婧
李亚静
刘志华
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Tianjin Chengjian University
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Tianjin Chengjian University
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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
    • C04B28/24Compositions 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 alkyl, ammonium or metal silicates; containing silica sols
    • 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
    • C04B20/00Use 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
    • C04B20/10Coating or impregnating
    • C04B20/1018Coating or impregnating with organic materials
    • C04B20/1022Non-macromolecular compounds
    • 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
    • C04B2201/20Mortars, concrete or artificial stone characterised by specific physical values for the density
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The present invention discloses a kind of natural halloysite clay aeroge for building heat preservation and preparation method thereof, and surface modification is carried out to natural galapectite;Tetraethyl orthosilicate, absolute ethyl alcohol, water are mixed, hydrochloric acid, the magnetic agitation under 25 DEG C 45 DEG C of water bath condition is added dropwise;Modified halloysite clay is evenly spread in absolute ethyl alcohol by ultrasonic vibration, ammoniacal liquor is instilled, stirs;Tetraethyl orthosilicate mixed liquor after hydrolysis is sufficiently mixed with halloysite clay suspension, the gel under conditions of 20 DEG C 50 DEG C, obtains halloysite clay wet gel;Dried 23 days under 50 DEG C of condition of normal pressure and obtain block-shaped target product.The clay soil clay soil silica aerogel of the present invention is applied to various building heat preservation structures, and anti-flammability is good, high-efficiency insulated energy-conservation.

Description

A kind of natural halloysite clay aeroge for building heat preservation and preparation method thereof
Technical field
The present invention relates to controllable natural clay aeroge of a kind of microscopic void and preparation method thereof, more specifically, relate to And a kind of halloysite clay aeroge heat-insulated for building heat preservation and preparation method thereof, it disclosure satisfy that the state of building thermal insulation material Family's standard requirement, belongs to building energy-saving heat-insulating material field.
Background technology
Building heat preservation industry is the market that tremendous potential be present in China, raising and section with building energy conservation requirement The development of energy technology, building heat preservation heat-barrier material also develop to lightweight, multi-functional and energy-conserving and environment-protective direction.Aerogel material conduct A kind of Performances of Novel Nano-Porous meter level lightweight, multi-functional, environment-friendly materials, are increasingly got more and more people's extensive concerning, especially with the property that its is unique It is the focus for being had become research as a kind of high-efficiency insulated heat-barrier material.On the one hand, consolidate as most light in the world Body-aeroge, useful up to 99% porosity, has good heat-insulating property, has with the insulation material prepared by it light Matter, thermal conductivity is low to wait premium properties, sufficiently meets energy-efficient requirement;On the other hand, conventional aeroge (such as two Silica aerogel, alumina aerogels etc.) good fire resistance is respectively provided with, this is other organic insulation material institutes such as polyphenyl It can not compare.Conventional SiO at present2Aeroge, hydrolysis is mainly passed through by presomas such as tetraethyl orthosilicate, multi-polysiloxanes Condensation, prepares block hydrogel, then obtain aeroge by supercritical drying.But due to its fragility height, low intensity, cost The defects of high, it is difficult to carry out large-scale industrial production, seriously constrain development of the aeroge in building heat preservation field.Therefore find A kind of brand-new aeroge raw material, prepare a kind of high intensity, fire-retardant rank it is high, it is cost-effective, available for large-scale industry The aeroge insulation material of production is current building heat preservation industry urgent problem to be solved.
The content of the invention
Instant invention overcomes traditional aeroge insulation material low intensity, fragility is big, production cost is high the defects of, it is therefore intended that One kind is provided and can apply to various building heat preservation structures, anti-flammability is good, and the novel clay soil aeroge of high-efficiency insulated energy-conservation is protected Adiabator and preparation method thereof.
The technical purpose of the present invention is achieved by following technical proposals:
A kind of natural halloysite clay aeroge for building heat preservation and preparation method thereof, is carried out as steps described below:
Step 1, tetraethyl orthosilicate, absolute ethyl alcohol, water are well mixed and concentrated hydrochloric acid is added dropwise, in 25 DEG C -45 DEG C of water-bath Under the conditions of magnetic agitation, the tetraethyl orthosilicate mixed liquor (i.e. halloysite clay crosslinking agent) for making it be fully hydrolyzed after being hydrolyzed;
In step 1, temperature is 30-40 degrees Celsius.
In step 1, magnetic agitation time at least 30min, preferably 1-3 hours.
In step 1, tetraethyl orthosilicate, water, the mass ratio of absolute ethyl alcohol are (4-5):(7—10):(1-2), preferably (4—5):(7—8):2.
In step 1, concentrated hydrochloric acid is the aqueous solution for the hydrogen chloride that mass percent is 30-35%, and dosage is added dropwise so that body It is pH stable 1-2, sour environment is provided for hydrolysis.
Step 2, modified halloysite clay is evenly spread in absolute ethyl alcohol by ultrasonic vibration and ammoniacal liquor is added dropwise and stirs Uniformly, to obtain suffering Lip river stone slurry, wherein it is (1-5) that Lip river stone clay and the mass ratio of absolute ethyl alcohol are suffered in modification:10, It is preferred that (1-2):10.
In step 2, ammoniacal liquor is the aqueous solution (NH for the ammonia that mass percent is 10-15%3+H2O), be added dropwise dosage so that System pH is stable 10-12, and alkaline environment is provided for halloysite clay suspension.
In step 2, when preparing halloysite clay suspension, select under the conditions of 100-200Hz ultrasound 10- 30min is obtained.
In step 2, modified halloysite clay is prepared by following methods:(1) by natural halloysite clay salt Acid solution is handled, and is cleaned;(2) the natural angstrom of Lip river handled using modifying agent isooctyltriethoxysilane step (1) Stone carries out that surface is modified simultaneously to be cleaned, wherein in step (1), concentration of hydrochloric acid be 1-5M, the mass parts of natural halloysite clay with The ratio of the parts by volume of hydrochloric acid solution is (1-3):(10-20), treatment temperature are 20-25 degrees Celsius, and processing time is 1-3 Hour;In step (2), the mass ratio of the natural galapectite of modifying agent isooctyltriethoxysilane and step (1) processing is (10—15):(3-5), the temperature of modified-reaction is 60-80 degrees Celsius, and the time is 1-5 hours.
Step 3, halloysite clay prepared by tetraethyl orthosilicate mixed liquor and step 2 after the hydrolysis prepared by step 1 hangs After supernatant liquid is sufficiently mixed, natural halloysite clay wet gel is obtained under the conditions of 20 DEG C-50 DEG C, in 50-60 DEG C of condition of normal pressure Natural halloysite clay aeroge is obtained after lower drying.
In step 3, halloysite clay prepared by tetraethyl orthosilicate mixed liquor and step 2 after the hydrolysis that prepared by step 1 The dosage of suspension for etc. mass parts.
Halloysite nanotubes (HNTs) are a kind of cheap natural nano pipes of well-crystallized, are often multi-walled pipes shape knot Structure, formed by alumina octahedral and the curling of silicon-oxy tetrahedron lattice mismatch, be a kind of clay with nano-scale fiber shape structure, The be modified halloysite nanotubes outer surface of modified can produce many active groups, this cause halloysite clay prepare it is high Possibility, and the owned good crystalline texture of galapectite on porosity building thermal insulation material be present, this is with its preparation Aerogel material has higher intensity than conventional silica-based aerogel.
Compared with prior art, the characteristics of new halloysite clay aeroge of the invention and advantage:(1) bat pattern.Two It is crosslinked between silica offspring ball and halloysite nanotubes between ball, forms galapectite by the filling of absolute ethyl alcohol One three-dimensional network architecture, also being understood as halloysite clay aeroge has uniform nanoscale microstructure, inside angstrom Lip river stone nanotube is randomly dispersed within three dimensions by silica crosslinking;(2) lightweight, high porosity, lower thermal conductivity.By dry After dry process removes absolute ethyl alcohol, material internal produces a large amount of nanoscales and micron-sized hole, and porosity is up to 90- 95%, average pore diameter is 0.8-1.2 μm, and pore volume is 2-2.2ml/g, and specific surface area is 740-780m2/ g, density exist 0.015-0.025g/cm3Between, thermal conductivity factor is in 0.025-0.040Wm-1·K-1In the range of, make halloysite clay aeroge Premium properties with ultra-light heat insulation;(3) microscopic dimensions are controllable.The microscopic voids structure of galapectite aeroge can pass through change The addition of crosslinking agent and the dosage of absolute ethyl alcohol regulate and control;(4) production cost is low.Raw material sources are wide, cheap, and drying is set It is standby to require low, in all kinds of building heat preservation components that can be widely applied.
Brief description of the drawings
Fig. 1 be the present invention before modified after halloysite nanotubes infrared spectrogram, wherein 1 is before modified, 2 is are modified Afterwards.Fig. 2 is the SEM pictures of modified galapectite in the present invention.
Fig. 3 is halloysite clay aeroge SEM pictures in the present invention.
Fig. 4 is halloysite clay aeroge TEM pictures in the present invention.
Fig. 5 is that halloysite clay aeroge three-dimensional structure builds schematic diagram in the present invention, wherein bar-shaped is galapectite, it is spherical For silica.
Embodiment
Technical scheme is further illustrated with reference to specific embodiment.
The natural galapectite of purchase is modified first, the raw material using modified galapectite as subsequent embodiment.
(1) natural halloysite clay is handled with hydrochloric acid solution, and cleaned, concentration of hydrochloric acid 1M, natural galapectite The ratio of the mass parts (g) of clay and the parts by volume (ml) of hydrochloric acid solution is 3:20, treatment temperature is 20-25 degrees Celsius, processing Time is 1 hour;
(2) the natural galapectite handled using modifying agent isooctyltriethoxysilane step (1) carries out surface modification, The mass ratio of modifying agent isooctyltriethoxysilane and the natural galapectite of step (1) processing is 15:3, the temperature of modified-reaction Spend for 70 degrees Celsius, the time is 2 hours.
The galapectite after before modified is characterized (in Fu of Thermo companies of U.S. Nicolet 380 using infrared spectrum Leaf transformation infrared spectrometer), as shown in Figure 1, occur obvious iso-octyl functional group, explanation on modified galapectite curve Galapectite is modified successful.The hydrochloric acid used in embodiment is the aqueous solution for the hydrogen chloride that mass percent is 30%, is made Ammoniacal liquor is the aqueous solution (NH for the ammonia that mass percent is 10%3+H2O)。
Embodiment 1
Step 1, tetraethyl orthosilicate, absolute ethyl alcohol, water are mixed by a certain percentage, 2 drop concentrated hydrochloric acids is added dropwise, in 35 DEG C of water Magnetic agitation under the conditions of bath, tetraethyl orthosilicate mixed liquor (the i.e. halloysite clay crosslinking for making it be fully hydrolyzed after being hydrolyzed Agent);Magnetic agitation time 30min;Tetraethyl orthosilicate, water, the mass ratio of absolute ethyl alcohol are 5:7:2;
Step 2,1g is modified halloysite clay to evenly spread in 10g absolute ethyl alcohol by ultrasonic vibration, instills 4 drops Ammoniacal liquor, the ultrasonic 10min under the conditions of 100Hz is selected, to obtain suffering Lip river stone slurry;
Step 3, by etc. quality hydrolysis after tetraethyl orthosilicate mixed liquor be sufficiently mixed with halloysite clay suspension, Gel under conditions of 35 DEG C, obtain halloysite clay wet gel;Dried under 50 DEG C of condition of normal pressure and obtain within 2 days block-shaped target production Product.
Embodiment 2
Step 1, tetraethyl orthosilicate, absolute ethyl alcohol, water are mixed by a certain percentage, 2 drop concentrated hydrochloric acids is added dropwise, in 40 DEG C of water Magnetic agitation under the conditions of bath, tetraethyl orthosilicate mixed liquor (the i.e. halloysite clay crosslinking for making it be fully hydrolyzed after being hydrolyzed Agent);Magnetic agitation time 1h;Tetraethyl orthosilicate, water, the mass ratio of absolute ethyl alcohol are 4:10:1;
Step 2,5g is modified halloysite clay to evenly spread in 10g absolute ethyl alcohol by ultrasonic vibration, instills 4 drops Ammoniacal liquor, the ultrasonic 30min under the conditions of 200Hz is selected, to obtain suffering Lip river stone slurry;
Step 3, by etc. quality hydrolysis after tetraethyl orthosilicate mixed liquor be sufficiently mixed with halloysite clay suspension, Gel under conditions of 20 DEG C, obtain halloysite clay wet gel;Dried under 60 DEG C of condition of normal pressure and obtain within 2 days block-shaped target production Product.
Embodiment 3
Step 1, tetraethyl orthosilicate, absolute ethyl alcohol, water are mixed by a certain percentage, 2 drop concentrated hydrochloric acids is added dropwise, in 30 DEG C of water Magnetic agitation under the conditions of bath, tetraethyl orthosilicate mixed liquor (the i.e. halloysite clay crosslinking for making it be fully hydrolyzed after being hydrolyzed Agent);Magnetic agitation time 3h;Tetraethyl orthosilicate, water, the mass ratio of absolute ethyl alcohol are 5:8:2;
Step 2,2g is modified halloysite clay to evenly spread in 10g absolute ethyl alcohol by ultrasonic vibration, instills 4 drops Ammoniacal liquor, the ultrasonic 20min under the conditions of 150Hz is selected, to obtain suffering Lip river stone slurry;
Step 3, by etc. quality hydrolysis after tetraethyl orthosilicate mixed liquor be sufficiently mixed with halloysite clay suspension, Gel under conditions of 50 DEG C, obtain halloysite clay wet gel;Dried under 55 DEG C of condition of normal pressure and obtain within 2 days block-shaped target production Product.
The microscopic appearance of aeroge is observed using JEOL JSM-7800F types SEM, such as accompanying drawing institute Show, halloysite clay aeroge has uniform nanoscale microstructure, and internal halloysite nanotubes are crosslinked nothing by silica Sequence is distributed in three dimensions.Using the N2 adsorption specific surface area measuring instrument (3H- of scientific and technological (Beijing) Co., Ltd of Bei Shide instruments 2000PS1) it is measured, a large amount of nanoscales and micron-sized hole are produced inside the aerogel material prepared by the present invention Gap, porosity are up to 90-95%, and average pore diameter is 0.8-1.2 μm, and pore volume is 2-2.2ml/g, and specific surface area is 740—780m2/ g, while use airsetting of Xi'an Xiatech Electronic Technology Co., Ltd. TC3000E types thermal conductivity factor instrument to preparation Glue product carries out the test of thermal conductivity factor, and thermal conductivity factor is average up to 0.015-0.02W/mK.
It is adjusted according to the technique that Summary is recorded, can prepares halloysite clay aeroge, after tested table Reveal property consistent with the above.
Exemplary description has been done to the present invention above, it should explanation, in the situation for the core for not departing from the present invention Under, any simple deformation, modification or other skilled in the art can not spend the equivalent substitution of creative work equal Fall into protection scope of the present invention.

Claims (10)

1. a kind of natural halloysite clay aeroge for building heat preservation, it is characterised in that carry out as steps described below:
Step 1, tetraethyl orthosilicate, absolute ethyl alcohol, water are well mixed and concentrated hydrochloric acid is added dropwise, in 25 DEG C -45 DEG C of water bath condition Lower magnetic agitation, the tetraethyl orthosilicate mixed liquor for making it be fully hydrolyzed after being hydrolyzed;Tetraethyl orthosilicate, water, absolute ethyl alcohol Mass ratio is (4-5):(7—10):(1—2);
Step 2, modified halloysite clay is evenly spread in absolute ethyl alcohol by ultrasonic vibration and ammoniacal liquor is added dropwise and stirs, To obtain suffering Lip river stone slurry, wherein it is (1-5) that Lip river stone clay and the mass ratio of absolute ethyl alcohol are suffered in modification:10;In step In 2, modified halloysite clay is prepared by following methods:(1) natural halloysite clay is handled with hydrochloric acid solution, And clean;(2) the natural galapectite handled using modifying agent isooctyltriethoxysilane step (1) carries out surface modification simultaneously Cleaning, wherein in step (1), the ratio of the mass parts of natural halloysite clay and the parts by volume of hydrochloric acid solution is (1-3): (10-20), treatment temperature are 20-25 degrees Celsius, and processing time is 1-3 hours;In step (2), modifying agent iso-octyl three The mass ratio of Ethoxysilane and the natural galapectite of step (1) processing is (10-15):(3-5), the temperature of modified-reaction are 60-80 degrees Celsius, the time is 1-5 hours;
Step 3, halloysite clay suspension prepared by tetraethyl orthosilicate mixed liquor and step 2 after the hydrolysis prepared by step 1 After being sufficiently mixed, natural halloysite clay wet gel is obtained under the conditions of 20 DEG C-50 DEG C, is done under 50-60 DEG C of condition of normal pressure Obtain natural halloysite clay aeroge after dry, a large amount of nanoscales and micron-sized are produced inside natural halloysite clay aeroge Hole, porosity are up to 90-95%, and average pore diameter is 0.8-1.2 μm, and pore volume is 2-2.2ml/g, and specific surface area is 740—780m2/ g, density is in 0.015-0.025g/cm3Between, thermal conductivity factor is in 0.025-0.040Wm-1·K-1
A kind of 2. natural halloysite clay aeroge for building heat preservation according to claim 1, it is characterised in that In step 1, tetraethyl orthosilicate, water, the mass ratio of absolute ethyl alcohol are (4-5):(7—8):2;Temperature is 30-40 degrees Celsius;Magnetic Power mixing time at least 30min, preferably 1-3 hours;Concentrated hydrochloric acid is the water-soluble of the hydrogen chloride that mass percent is 30-35% Liquid, dosage is added dropwise so that system pH stabilization provides sour environment 1-2, for hydrolysis.
A kind of 3. natural halloysite clay aeroge for building heat preservation according to claim 1, it is characterised in that In step 2, it is (1-2) to be modified and suffer Lip river stone clay and the mass ratio of absolute ethyl alcohol:10;Ammoniacal liquor be mass percent be 10- The aqueous solution (the NH of 15% ammonia3+H2O), dosage is added dropwise so that system pH is stable 10-12, is halloysite clay suspension Alkaline environment is provided;When preparing halloysite clay suspension, 10-30min of ultrasound under the conditions of 100-200Hz is selected to obtain Arrive.
A kind of 4. natural halloysite clay aeroge for building heat preservation according to claim 1, it is characterised in that In step 3, the use of halloysite clay suspension prepared by tetraethyl orthosilicate mixed liquor and step 2 after hydrolysis prepared by step 1 Measure for etc. mass parts.
5. the preparation method of a kind of natural halloysite clay aeroge for building heat preservation, it is characterised in that according to following steps It is rapid to carry out:
Step 1, tetraethyl orthosilicate, absolute ethyl alcohol, water are well mixed and concentrated hydrochloric acid is added dropwise, in 25 DEG C -45 DEG C of water bath condition Lower magnetic agitation, the tetraethyl orthosilicate mixed liquor for making it be fully hydrolyzed after being hydrolyzed;Tetraethyl orthosilicate, water, absolute ethyl alcohol Mass ratio is (4-5):(7—10):(1—2);
Step 2, modified halloysite clay is evenly spread in absolute ethyl alcohol by ultrasonic vibration and ammoniacal liquor is added dropwise and stirs, To obtain suffering Lip river stone slurry, wherein it is (1-5) that Lip river stone clay and the mass ratio of absolute ethyl alcohol are suffered in modification:10;In step In 2, modified halloysite clay is prepared by following methods:(1) natural halloysite clay is handled with hydrochloric acid solution, And clean;(2) the natural galapectite handled using modifying agent isooctyltriethoxysilane step (1) carries out surface modification simultaneously Cleaning, wherein in step (1), the ratio of the mass parts of natural halloysite clay and the parts by volume of hydrochloric acid solution is (1-3): (10-20), treatment temperature are 20-25 degrees Celsius, and processing time is 1-3 hours;In step (2), modifying agent iso-octyl three The mass ratio of Ethoxysilane and the natural galapectite of step (1) processing is (10-15):(3-5), the temperature of modified-reaction are 60-80 degrees Celsius, the time is 1-5 hours;
Step 3, halloysite clay suspension prepared by tetraethyl orthosilicate mixed liquor and step 2 after the hydrolysis prepared by step 1 After being sufficiently mixed, natural halloysite clay wet gel is obtained under the conditions of 20 DEG C-50 DEG C, is done under 50-60 DEG C of condition of normal pressure Natural halloysite clay aeroge is obtained after dry.
6. a kind of preparation method of natural halloysite clay aeroge for building heat preservation according to claim 5, its It is characterised by, in step 1, tetraethyl orthosilicate, water, the mass ratio of absolute ethyl alcohol are (4-5):(7—8):2;Temperature be 30- 40 degrees Celsius;The magnetic agitation time at least 30min, preferably 1-3 hours.
7. a kind of preparation method of natural halloysite clay aeroge for building heat preservation according to claim 5, its Be characterised by, in step 1, concentrated hydrochloric acid is the aqueous solution for the hydrogen chloride that mass percent is 30-35%, be added dropwise dosage so that System pH is stable 1-2, and sour environment is provided for hydrolysis.
8. a kind of preparation method of natural halloysite clay aeroge for building heat preservation according to claim 5, its It is characterised by, in step 2, it is (1-2) to be modified and suffer Lip river stone clay and the mass ratio of absolute ethyl alcohol:10;Ammoniacal liquor is quality percentage Number is the aqueous solution (NH of 10-15% ammonia3+H2O), dosage is added dropwise so that system pH is stable 10-12, is glued for galapectite Native suspension provides alkaline environment;When preparing halloysite clay suspension, select under the conditions of 100-200Hz ultrasound 10- 30min is obtained.
9. a kind of preparation method of natural halloysite clay aeroge for building heat preservation according to claim 5, its It is characterised by, in step 3, halloysite clay prepared by tetraethyl orthosilicate mixed liquor and step 2 after hydrolysis prepared by step 1 The dosage of suspension for etc. mass parts.
10. natural application of the halloysite clay aeroge in building heat preserving as claimed in claim 1.
CN201610779233.5A 2016-08-31 2016-08-31 A kind of natural halloysite clay aeroge for building heat preservation and preparation method thereof Pending CN107777979A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109897371A (en) * 2019-03-15 2019-06-18 成都新柯力化工科技有限公司 A kind of the environment-friendly type flame-retardant plastic masterbatch and preparation method of anti-precipitation
CN111909418A (en) * 2020-08-17 2020-11-10 吉林大学 Modified polyimide aerogel and preparation method and application thereof
CN115650643A (en) * 2022-09-26 2023-01-31 江苏泰林建设有限公司 Light self preservation temperature haydite board

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006127572A2 (en) * 2005-05-20 2006-11-30 Technology Innovations, Llc Ultracapacitors comprised of mineral microtubules
CN105565774A (en) * 2015-05-11 2016-05-11 天津城建大学 High-strength high-thermal-insulation silica aerogel and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2006127572A2 (en) * 2005-05-20 2006-11-30 Technology Innovations, Llc Ultracapacitors comprised of mineral microtubules
CN105565774A (en) * 2015-05-11 2016-05-11 天津城建大学 High-strength high-thermal-insulation silica aerogel and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
HONGLI LIU等: "Novel three-dimensional halloysite nanotubes/silica composite aerogels with enhanced mechanical strength and low thermal conductivity prepared at ambient pressure", 《JOURNAL OF SOL-GEL SCIENCE AND TECHNOLOGY》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109897371A (en) * 2019-03-15 2019-06-18 成都新柯力化工科技有限公司 A kind of the environment-friendly type flame-retardant plastic masterbatch and preparation method of anti-precipitation
CN109897371B (en) * 2019-03-15 2021-05-07 佛山市碧坤塑料有限公司 Precipitation-proof environment-friendly flame-retardant plastic master batch and preparation method thereof
CN111909418A (en) * 2020-08-17 2020-11-10 吉林大学 Modified polyimide aerogel and preparation method and application thereof
CN115650643A (en) * 2022-09-26 2023-01-31 江苏泰林建设有限公司 Light self preservation temperature haydite board

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Application publication date: 20180309