CN106430220A - Method for preparing silicon dioxide aerogel from quartz tailings as raw material - Google Patents
Method for preparing silicon dioxide aerogel from quartz tailings as raw material Download PDFInfo
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- CN106430220A CN106430220A CN201610814111.5A CN201610814111A CN106430220A CN 106430220 A CN106430220 A CN 106430220A CN 201610814111 A CN201610814111 A CN 201610814111A CN 106430220 A CN106430220 A CN 106430220A
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- hydrogel
- aerosil
- raw material
- tail sand
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 217
- 239000010453 quartz Substances 0.000 title claims abstract description 72
- 238000000034 method Methods 0.000 title claims abstract description 48
- 239000002994 raw material Substances 0.000 title claims abstract description 45
- 235000012239 silicon dioxide Nutrition 0.000 title abstract description 69
- 239000000377 silicon dioxide Substances 0.000 title abstract description 12
- 239000004964 aerogel Substances 0.000 title abstract description 11
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 98
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000017 hydrogel Substances 0.000 claims abstract description 61
- 239000000047 product Substances 0.000 claims abstract description 28
- 239000000499 gel Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 19
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 18
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 18
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 239000000706 filtrate Substances 0.000 claims abstract description 3
- 239000004576 sand Substances 0.000 claims description 65
- 238000005406 washing Methods 0.000 claims description 51
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 49
- 238000010521 absorption reaction Methods 0.000 claims description 45
- 238000006073 displacement reaction Methods 0.000 claims description 41
- 230000032683 aging Effects 0.000 claims description 34
- 238000004140 cleaning Methods 0.000 claims description 16
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 239000011812 mixed powder Substances 0.000 claims description 16
- 238000002791 soaking Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 13
- 239000003292 glue Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 8
- 230000002209 hydrophobic effect Effects 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000002360 preparation method Methods 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 abstract 2
- 230000002431 foraging effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000005051 trimethylchlorosilane Substances 0.000 abstract 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 241000790917 Dioxys <bee> Species 0.000 description 7
- 229910003978 SiClx Inorganic materials 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 229910018540 Si C Inorganic materials 0.000 description 6
- 229910008051 Si-OH Inorganic materials 0.000 description 6
- 229910006358 Si—OH Inorganic materials 0.000 description 6
- 238000012512 characterization method Methods 0.000 description 6
- 238000001514 detection method Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 239000011148 porous material Substances 0.000 description 6
- 229910010271 silicon carbide Inorganic materials 0.000 description 6
- 239000006004 Quartz sand Substances 0.000 description 4
- 239000004965 Silica aerogel Substances 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 241001274660 Modulus Species 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- -1 butyl silicates Chemical class 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a method for preparing silicon dioxide aerogel from quartz tailings as a raw material. The method comprises the following steps: step 1, the quartz tailings are washed, dried, ground and sieved and then ground and mixed with sodium carbonate powder, a mixture is calcined, and a calcination product is obtained; step 2, the calcination product is ground and sieved, undersized matter is added to hot water to be stirred and dissolved, the solution is filtered, a filtrate is taken, and water glass is obtained; step 3, the pH value of the water glass is regulated with hydrochloric acid, a sol-gel reaction is performed, a product is left to stand for aging, and hydrogel is obtained; step 4, free water in the hydrogel is filtered out, residual moisture is replaced with absolute ethyl alcohol, and alcogel is obtained; step 5, the alcogel is soaked with an n-hexane solution of trimethylchlorosilane, and hydrophobically modified alkane gel is obtained; step 6, drying is performed, and the silicon dioxide aerogel is obtained. The raw materials are cheap and available, the preparation process adopts mild conditions and has low equipment requirements, so that the production cost of the silicon dioxide aerogel is reduced greatly, and the prepared aerogel has good performance.
Description
Technical field
The invention belongs to aerosil technical field, and in particular to one kind prepares dioxy with quartz tail sand as raw material
The method of SiClx aeroge.
Background technology
Aerosil is made up of nanoscale hole hole and silica inorganic polymer three-dimensional nano bone frame, high hole
Rate, may be up to 99.8%；High-specific surface area, may be up to 1000m2/ more than g；Low-density, can as little as 0.003g/cm3.There is refraction
The advantages of rate is low, Young's moduluss are little, acoustic impedance is low, heat conductivity is low and absorption property is strong, chemistry, calorifics, optics, acoustics,
The aspects such as electricity show peculiar property, have extensively in numerous areas such as space flight, military project, communication, medical, building materials, electronics, metallurgy
Wealthy application prospect.But the production of aerosil is many with Organic substances such as tetraethyl orthosilicate, butyl silicates as silicon at present
Source, through sol gel reaction, supercritical drying is obtained.This method cost of material height, preparation process condition harshness, to equipment requirements
High, dangerous big, cause the cost of aerosil extremely expensive, so as to significantly limit which in the wide of numerous areas
General application.So, it is that aerosil can be extensive to seek cheap raw material and gently cheap manufacturing condition
Application, plays premise and the key of its premium properties.
Quartz tail sand, is the garbage of the raw material quartz sand for producing glass, can corrode as the silica flour of particulate enters furnace rear
Refractory material, reduces the life-span of melting furnaces, affects the uniformity of batch, while also checker brick passage can be blocked, is unfavorable for glass
Production, therefore glass industry is to be greater than 95% between the granule content of 0.125mm to 0.71mm to the granularity requirements of quartz sand,
Quartzy powder content less than 0.125mm is less than 5%.Quartz sand manufacturing enterprise is for the quartzy fine powder less than below 0.125mm
Most of not recycling, but concentrate and pile up discharge.The bulk deposition of Quartz Tails, not only defines the wasting of resources, also
Large area soil is taken, soil is destroyed, due to its superfine characteristic, " meeting water to be lost in, air-dry and fly upward ", easily form mudstone
The natural disasters such as stream, sandstorm, seriously jeopardize ecological environment and the people's lives and property safety.So, it would be highly desirable to seek efficiently comprehensive
The outlet that utilizes is closed, to turn waste into wealth, eliminates that its idle heap is rivals in a contest natural environment and that people life property safety causes is huge
Hidden danger.
Content of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, provides one kind with quartz tail sand
For the method that raw material prepares aerosil.The method raw material is cheap and easy to get, and preparation process condition is gentle, to equipment requirements
Low, so that the production cost of aerosil is substantially reduced, and obtained aeroge has good performance；With
When, high value added utilization of the method to quartz tail sand, can eliminate which brings to environment and people life property safety is huge
Big hidden danger；Also can achieve quartz mine is used for Poly-generation and the sustainable development of glass and aerosil product.
For solving above-mentioned technical problem, the technical solution used in the present invention is：One kind prepares two with quartz tail sand as raw material
The method of silica aerogel, it is characterised in that the method is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, process of drying, grind and sieve, quartz tail sand powder is obtained, so
Afterwards by the quartz tail sand powder and powdered sodium carbonate (0.8～1.6) in mass ratio: 1 ground and mixed, mixed-powder is obtained, it
Afterwards the mixed-powder is placed in Muffle furnace and calcines, obtain calcined product；
Step 2, will calcined product described in step one grind after sieve, extracting screen underflow, then by the siftage add
To in hot water, stirring and dissolving 60min～150min, filters to take filtrate afterwards, obtains waterglass；The matter of the siftage and hot water
Amount is than being 1: (3～5)；
Step 3, using hydrochloric acid, the pH value of waterglass described in step 2 is adjusted to 3～5, after standing 20min～50min
Obtain hydrogel, then by the hydrogel temperature be 40 DEG C～60 DEG C under conditions of aging 3d～5d, obtain aging after
Hydrogel；
Step 4, the hydrogel after aging described in step 3 is filtered, to remove the Free water in hydrogel, so
Afterwards line replacement is entered to residuing in hydrogel surface and the absorption water in hole using dehydrated alcohol, obtain alcogel；
Step 5, alcogel described in step 4 is soaked in the hexane solution of trim,ethylchlorosilane, to be dredged
Modified and displacement of the normal hexane to ethanol of water, obtains the alkane gel of hydrophobically modified after washing；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；In the gradient dried process, the temperature of each stage dried according to
Secondary is 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, and the time of each stage dried is 3h～5h.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step one
Described in ground and mixed time be 30min.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step one
Described in the temperature calcined be 1100 DEG C～1400 DEG C, time of the calcining be.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 2
Described in hot water temperature be 60 DEG C～90 DEG C.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 3
Described in hydrochloric acid concentration be 0.1mol/L～0.5mol/L.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 4
Described in the number of times replaced be 3～6 times, every time the volume of displacement dehydrated alcohol used is 1～6 times of hydrogel volume, per
Secondary displacement is all carried out under conditions of temperature is 30 DEG C～50 DEG C, and the time that replaces every time is 3h～5h.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 4
Described in filter during the hydrogel after aging is washed as cleaning mixture using deionized water, the washing time
Number is 3～4 times, every time the volume of washing institute deionized water be aging after 2～3 times of hydrogel volume.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 5
Described in the number of times that soaks be 3～5 times, the volume for soaking every time the hexane solution of trim,ethylchlorosilane used is alcogel
1～6 times of volume, soaking every time is all carried out under conditions of temperature is 20 DEG C～40 DEG C, the time that soaks every time be 3h～
5h.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 5
Described in trim,ethylchlorosilane hexane solution in trim,ethylchlorosilane weight/mass percentage composition be 6%～10%.
A kind of above-mentioned method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that step 5
Described in wash the cleaning mixture of employing be normal hexane, the number of times of the washing be 3～5 times, every time washing normal hexane used body
Product is 2～3 times of alcogel volume.
The present invention has advantages below compared with prior art：
1st, raw material of the present invention is cheap and easy to get, the raw materials used garbage quartz tail sand for glass industry, but not limited to this,
It can be general quartz sand raw material；
2nd, the present invention is dry by the gradient temperature under normal pressure, low for equipment requirements, safety, and it is convenient to realize, easy to operate；
3rd, there is the quartz tail sand of huge environment and potential safety hazard in efficient utilization of the present invention, be that the height of quartz tail sand is added
Value is utilized and opens new outlet；
4th, the present invention can realize quartz mine for producing the Poly-generation of glass and aeroge；
5th, aerosil function admirable prepared by the present invention.
In a word, raw material of the present invention is cheap and easy to get, and preparation process condition is gentle, low for equipment requirements, so that titanium dioxide
The production cost of silica aerogel is substantially reduced, and obtained aeroge has good performance.While the method is to quartz tail sand
High value added utilization, its huge hidden danger brought by environment and people life property safety can be eliminated；Also quartz can achieve
Mining Poly-generation and sustainable development in glass and aerosil product.
With reference to embodiment, the present invention is described in further detail.
Specific embodiment
Embodiment 1
The method that the present embodiment prepares aerosil with quartz tail sand as raw material is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, drying, grinding and cross 325 mesh sieves process, obtain quartz tail sand powder
End, then by the quartz tail sand powder and powdered sodium carbonate 1.2: 1 ground and mixed 30min in mass ratio, obtains mixed-powder,
Afterwards the mixed-powder being placed in Muffle furnace, 120min is calcined under conditions of temperature is 1100 DEG C, obtain calcined product；
Step 2, will calcined product described in step one grind after cross 200 mesh sieves, extracting screen underflow, then by described sieve under
Thing is added to stirring and dissolving 120min in the hot water that temperature is 80 DEG C, obtains waterglass after filtration；The siftage and hot water
Mass ratio is 1: 3；
The pH value of waterglass described in step 2 is adjusted to 4 by step 3, the hydrochloric acid using concentration for 0.2mol/L, standing
Obtain hydrogel after 30min, then by the hydrogel temperature be 40 DEG C under conditions of aging 4d, obtain aging after water-setting
Glue；
Step 4, be filtered to remove aging described in step 3 after hydrogel in Free water, then adopt dehydrated alcohol
To residue in hydrogel show and hole in absorption water enter line replacement, obtain alcogel；The number of times of the displacement is 3 times, per
Used by secondary displacement, the volume of dehydrated alcohol is 6 times of hydrogel volume, and the temperature of displacement is 40 DEG C every time, each displacement
Time is 4h；As cleaning mixture, the hydrogel after aging is washed using deionized water during filtration, described wash
The number of times that washs is 3 times, and the volume of washing institute deionized water is 3 times of hydrogel volume every time；
Alcogel described in step 5, the hexane solution soaking step four using trim,ethylchlorosilane, hydrophobic to carry out
The displacement of modified and normal hexane, obtains the alkane gel of hydrophobically modified after washing；The number of times of the immersion is 3 times, soaks every time used
The volume of the hexane solution of trim,ethylchlorosilane is 5 times of alcogel volume, and the temperature for soaking displacement every time is 30 DEG C,
The time that soaks every time is 5h；The weight/mass percentage composition of trim,ethylchlorosilane in the hexane solution of the trim,ethylchlorosilane
For 10%；The cleaning mixture of the washing employing is normal hexane, and the number of times of the washing is 5 times, every time normal hexane used by washing
Volume is 2 times of the volume of gel；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；The temperature that during the gradient dried, each stage dries is successively
For 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time that each stage dries is 3h.
To the test characterization result of the aerosil that the present embodiment is prepared with quartz tail sand as raw material it is：Infrared light
Spectrogram shows, in 1092cm-1、811cm-1、465cm-1The strong peak at place is the characteristic absorption of Si-O-Si, and prepared dioxy is described
SiClx Aerogel bodies are Si-O-Si network skeleton structure；In 3433cm-1And 1645cm-1Pole weak peak for H-OH feature inhale
Receive, the absorption aqueouss very little of aeroge is described；1250cm-1、841cm-1、756cm-1The strong peak at place is Si-C characteristic absorption,
2934cm-1、1457cm-1、973cm-1Locate as-CH3Characteristic absorption, illustrate that aeroge surface has substantial amounts of-CH3, and
955cm-1The Si-OH characteristic absorption at place is very weak, illustrates-OH the overwhelming majority in aeroge by-Si (CH3)3Replace.For water
Contact angle reach 121 °, show that hydrophobicity is preferable.XRD tests made aeroge collection of illustrative plates and shows at 2 θ angles are 20～25 °
An existing disperse peak, illustrates made aeroge for amorphous material.Density and N2Absorption detection shows, made prepared silicon dioxide airsetting
The density of glue is 0.06g/cm3, BET surface area 762m2/g；Main distribution 10nm in aperture～90nm, average pore size 20nm.
Embodiment 2
The method that the present embodiment prepares aerosil with quartz tail sand as raw material is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, drying, grinding and cross 325 mesh sieves process, obtain quartz tail sand powder
End, then by the quartz tail sand powder and powdered sodium carbonate 1.4: 1 ground and mixed 30min in mass ratio, obtains mixed-powder,
Afterwards the mixed-powder being placed in Muffle furnace, 90min is calcined under conditions of temperature is 1200 DEG C, obtain calcined product；
Step 2, will calcined product described in step one grind after cross 200 mesh sieves, extracting screen underflow, then by described sieve under
Thing is added to stirring and dissolving 120min in the hot water that temperature is 70 DEG C, obtains waterglass after filtration；The siftage and hot water
Mass ratio is 1: 4；
The pH value of waterglass described in step 2 is adjusted to 3 by step 3, the hydrochloric acid using concentration for 0.3mol/L, standing
Obtain hydrogel after 20min, then by the hydrogel temperature be 60 DEG C under conditions of aging 3d, obtain aging after water-setting
Glue；
Step 4, be filtered to remove aging described in step 3 after hydrogel in Free water, then adopt dehydrated alcohol
Line replacement is entered to the absorption water for residuing in hydrogel hole, obtains alcogel；The number of times of the displacement is 6 times, replaces every time
The volume of dehydrated alcohol used is 1 times of hydrogel volume, and the temperature of displacement is 30 DEG C every time, and the time of displacement is equal every time
For 5h；Hydrogel after aging is washed as cleaning mixture using deionized water during filtration, the washing time
Number is 4 times, and the volume of washing institute deionized water is 2 times of hydrogel volume every time；
Alcogel described in step 5, the hexane solution soaking step four using trim,ethylchlorosilane, hydrophobic to carry out
The displacement of modified and normal hexane, obtains the alkane gel of hydrophobically modified after washing；The number of times of the immersion is 3 times, soaks every time used
The volume of the hexane solution of trim,ethylchlorosilane is 6 times of alcogel volume, and the temperature for soaking displacement every time is 40 DEG C,
The time that soaks every time is 5h；The weight/mass percentage composition of trim,ethylchlorosilane in the hexane solution of the trim,ethylchlorosilane
For 6%；The cleaning mixture that the washing is adopted is normal hexane, and the number of times of the washing is 5 times, every time the body of washing normal hexane used
Product is 2 times of the volume of gel；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；The temperature that during the gradient dried, each stage dries is successively
For 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time that each stage dries is 5h.
To the test characterization result of the aerosil that the present embodiment is prepared with quartz tail sand as raw material it is：Infrared light
Spectrogram shows, in 1091cm-1、815cm-1、467cm-1The strong peak at place is the characteristic absorption of Si-O-Si, and prepared dioxy is described
SiClx Aerogel bodies are Si-O-Si network skeleton structure；In 3428cm-1And 1641cm-1Pole weak peak for H-OH feature inhale
Receive, the absorption aqueouss very little of aeroge is described；1255cm-1、843cm-1、756cm-1The strong peak at place is Si-C characteristic absorption,
2929cm-1、1450cm-1、977cm-1Locate as-CH3Characteristic absorption, illustrate that aeroge surface has substantial amounts of-CH3, and
958cm-1The Si-OH characteristic absorption at place is very weak, illustrates-OH the overwhelming majority in aeroge by-Si (CH3)3Replace.For water
Contact angle reach 117 °, show that hydrophobicity is preferable.XRD tests made aeroge collection of illustrative plates and shows at 2 θ angles are 20～25 °
An existing disperse peak, illustrates made aeroge for amorphous material.Density and N2Absorption detection shows, made prepared silicon dioxide airsetting
The density of glue is 0.09g/cm3, BET surface area 725m2/g；Main distribution 20nm in aperture～90nm, average pore size 35nm.
Embodiment 3
The method that the present embodiment prepares aerosil with quartz tail sand as raw material is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, drying, grinding and cross 325 mesh sieves process, obtain quartz tail sand powder
End, then by the quartz tail sand powder and powdered sodium carbonate 1.5: 1 ground and mixed 30min in mass ratio, obtains mixed-powder,
Afterwards the mixed-powder being placed in Muffle furnace, 120min is calcined under conditions of temperature is 1300 DEG C, obtain calcined product；
Step 2, will calcined product described in step one grind after cross 200 mesh sieves, extracting screen underflow, then by described sieve under
Thing is added to stirring and dissolving 150min in the hot water that temperature is 60 DEG C, obtains waterglass after filtration；The siftage and hot water
Mass ratio is 1: 5；
The pH value of waterglass described in step 2 is adjusted to 5 by step 3, the hydrochloric acid using concentration for 0.5mol/L, standing
Obtain hydrogel after 50min, then by the hydrogel temperature be 40 DEG C under conditions of aging 5d, obtain aging after water-setting
Glue；
Step 4, be filtered to remove aging described in step 3 after hydrogel in Free water, then adopt dehydrated alcohol
Line replacement is entered to the absorption water for residuing in hydrogel hole, obtains alcogel；The number of times of the displacement is 3 times, replaces every time
The volume of dehydrated alcohol used is 6 times of hydrogel volume, and the temperature of displacement is 30 DEG C every time, and the time of displacement is equal every time
For 5h；Hydrogel after aging is washed as cleaning mixture using deionized water during filtration, the washing time
Number is 3 times, and the volume of washing institute deionized water is 2 times of hydrogel volume every time；
Alcogel described in step 5, the hexane solution soaking step four using trim,ethylchlorosilane, hydrophobic to carry out
The displacement of modified and normal hexane, obtains the alkane gel of hydrophobically modified after washing；The number of times of the immersion is 3 times, soaks every time used
The volume of the hexane solution of trim,ethylchlorosilane is 6 times of alcogel volume, and the temperature for soaking displacement every time is 20 DEG C,
The time that soaks every time is 5h；The weight/mass percentage composition of trim,ethylchlorosilane in the hexane solution of the trim,ethylchlorosilane
For 8%；The cleaning mixture that the washing is adopted is normal hexane, and the number of times of the washing is 3 times, every time the body of washing normal hexane used
Product is 3 times of the volume of gel；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；The temperature that during the gradient dried, each stage dries is successively
For 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time that each stage dries is 4h.
To the test characterization result of the aerosil that the present embodiment is prepared with quartz tail sand as raw material it is：Infrared light
Spectrogram shows, in 1089cm-1、809cm-1、467cm-1The strong peak at place is the characteristic absorption of Si-O-Si, and prepared dioxy is described
SiClx Aerogel bodies are Si-O-Si network skeleton structure；In 3429cm-1And 1644cm-1Pole weak peak for H-OH feature inhale
Receive, the absorption aqueouss very little of aeroge is described；1252cm-1、838cm-1、753cm-1The strong peak at place is Si-C characteristic absorption,
2936cm-1、1455cm-1、975cm-1Locate as-CH3Characteristic absorption, illustrate that aeroge surface has substantial amounts of-CH3, and
958cm-1The Si-OH characteristic absorption at place is very weak, illustrates-OH the overwhelming majority in aeroge by-Si (CH3)3Replace.For water
Contact angle reach 125 °, show that hydrophobicity is preferable.XRD tests made aeroge collection of illustrative plates and shows at 2 θ angles are 20～25 °
An existing disperse peak, illustrates made aeroge for amorphous material.Density and N2Absorption detection shows, made prepared silicon dioxide airsetting
The density of glue is 0.08g/cm3, BET surface area 879m2/g；Main distribution 5nm in aperture～60nm, average pore size 15nm.
Embodiment 4
The method that the present embodiment prepares aerosil with quartz tail sand as raw material is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, drying, grinding and cross 325 sieves process, obtain quartz tail sand powder
End, then by the quartz tail sand powder and powdered sodium carbonate 0.8: 1 ground and mixed 30min in mass ratio, obtains mixed-powder,
Afterwards the mixed-powder being placed in Muffle furnace, 90min is calcined under conditions of temperature is 1100 DEG C, obtain calcined product；
Step 2, will calcined product described in step one grind after cross 200 mesh sieves, extracting screen underflow, then by described sieve under
Thing is added to stirring and dissolving 150min in the hot water that temperature is 70 DEG C, obtains waterglass after filtration；The siftage and hot water
Mass ratio is 1: 3；
The pH value of waterglass described in step 2 is adjusted to 3 by step 3, the hydrochloric acid using concentration for 0.1mol/L, standing
Obtain hydrogel after 20min, then by the hydrogel temperature be 40 DEG C under conditions of aging 5d, obtain aging after water-setting
Glue；
Step 4, be filtered to remove aging described in step 3 after hydrogel in Free water, then adopt dehydrated alcohol
Enter line replacement to residuing in hydrogel surface and the absorption water in hole, obtain alcogel；The number of times of the displacement is 3 times, per
Used by secondary displacement, the volume of dehydrated alcohol is 6 times of hydrogel volume, and the temperature of displacement is 50 DEG C every time, each displacement
Time is 4h；As cleaning mixture, the hydrogel after aging is washed using deionized water during filtration, described wash
The number of times that washs is 4 times, and the volume of washing institute deionized water is 2 times of hydrogel volume every time；
Alcogel described in step 5, the hexane solution soaking step four using trim,ethylchlorosilane, hydrophobic to carry out
The displacement of modified and normal hexane, obtains the alkane gel of hydrophobically modified after washing；The number of times of the immersion is 5 times, soaks every time used
The volume of the hexane solution of trim,ethylchlorosilane is 5 times of alcogel volume, and the temperature for soaking displacement every time is 30 DEG C,
The time that soaks every time is 4h；The weight/mass percentage composition of trim,ethylchlorosilane in the hexane solution of the trim,ethylchlorosilane
For 7%；The cleaning mixture that the washing is adopted is normal hexane, and the number of times of the washing is 4 times, every time the body of washing normal hexane used
Product is 2 times of the volume of gel；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；The temperature that during the gradient dried, each stage dries is successively
For 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time that each stage dries is 5h.
To the test characterization result of the aerosil that the present embodiment is prepared with quartz tail sand as raw material it is：Infrared light
Spectrogram shows, in 1096cm-1、814cm-1、459cm-1The strong peak at place is the characteristic absorption of Si-O-Si, and prepared dioxy is described
SiClx Aerogel bodies are Si-O-Si network skeleton structure；In 3435cm-1And 1646cm-1Pole weak peak for H-OH feature inhale
Receive, the absorption aqueouss very little of aeroge is described；1250cm-1、841cm-1、752cm-1The strong peak at place is Si-C characteristic absorption,
2928cm-1、1461cm-1、969cm-1Locate as-CH3Characteristic absorption, illustrate that aeroge surface has substantial amounts of-CH3, and
957cm-1The Si-OH characteristic absorption at place is very weak, illustrates-OH the overwhelming majority in aeroge by-Si (CH3)3Replace.For water
Contact angle reach 128 °, show that hydrophobicity is preferable.XRD tests made aeroge collection of illustrative plates and shows at 2 θ angles are 20～25 °
An existing disperse peak, illustrates made aeroge for amorphous material.Density and N2Absorption detection shows, made prepared silicon dioxide airsetting
The density of glue is 0.06g/cm3, BET surface area 787m2/g；Main distribution 10nm in aperture～90nm, average pore size 30nm.
Embodiment 5
The method that the present embodiment prepares aerosil with quartz tail sand as raw material is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, drying, grinding and cross 325 mesh sieves process, obtain quartz tail sand powder
End, then by the quartz tail sand powder and powdered sodium carbonate 1.6: 1 ground and mixed 30min in mass ratio, obtains mixed-powder,
Afterwards the mixed-powder being placed in Muffle furnace, 150min is calcined under conditions of temperature is 1400 DEG C, obtain calcined product；
Step 2, will calcined product described in step one grind after cross 200 mesh sieves, extracting screen underflow, then by described sieve under
Thing is added to stirring and dissolving 120min in the hot water that temperature is 90 DEG C, obtains waterglass after filtration；The siftage and hot water
Mass ratio is 1: 4；
The pH value of waterglass described in step 2 is adjusted to 5 by step 3, the hydrochloric acid using concentration for 0.4mol/L, standing
Obtain hydrogel after 50min, then by the hydrogel temperature be 60 DEG C under conditions of aging 3d, obtain aging after water-setting
Glue；
Step 4, be filtered to remove aging described in step 3 after hydrogel in Free water, then adopt dehydrated alcohol
Enter line replacement to residuing in hydrogel surface and the absorption water in hole, obtain alcogel；The number of times of the displacement is 5 times, per
Used by secondary displacement, the volume of dehydrated alcohol is 4 times of hydrogel volume, and the temperature of displacement is 30 DEG C every time, each displacement
Time is 5h；As cleaning mixture, the hydrogel after aging is washed using deionized water during filtration, described wash
The number of times that washs is 3 times, and the volume of washing institute deionized water is 3 times of hydrogel volume every time；
Alcogel described in step 5, the hexane solution soaking step four using trim,ethylchlorosilane, hydrophobic to carry out
The displacement of modified and normal hexane, obtains the alkane gel of hydrophobically modified after washing；The number of times of the immersion is 4 times, soaks every time used
The volume of the hexane solution of trim,ethylchlorosilane is 5 times of alcogel volume, and the temperature for soaking displacement every time is 30 DEG C,
The time that soaks every time is 3h；The weight/mass percentage composition of trim,ethylchlorosilane in the hexane solution of the trim,ethylchlorosilane
For 9%；The cleaning mixture that the washing is adopted is normal hexane, and the number of times of the washing is 3 times, every time the body of washing normal hexane used
Product is 3 times of the volume of gel；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；The temperature that during the gradient dried, each stage dries is successively
For 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time that each stage dries is 3h.
To the test characterization result of the aerosil that the present embodiment is prepared with quartz tail sand as raw material it is：Infrared light
Spectrogram shows, in 1108cm-1、807cm-1、464cm-1The strong peak at place is the characteristic absorption of Si-O-Si, and prepared dioxy is described
SiClx Aerogel bodies are Si-O-Si network skeleton structure；In 3433cm-1And 1643cm-1The pole weak peak at place is the feature of H-OH
Absorb, the absorption aqueouss very little of aeroge is described；1250cm-1、842cm-1、753cm-1The strong peak at place is Si-C characteristic absorption,
2934cm-1、1456cm-1、972cm-1Locate as-CH3Characteristic absorption, illustrate that aeroge surface has substantial amounts of-CH3, and
952cm-1The Si-OH characteristic absorption at place is very weak, illustrates-OH the overwhelming majority in aeroge by-Si (CH3)3Replace.For water
Contact angle reach 110 °, show that hydrophobicity is preferable.XRD tests made aeroge collection of illustrative plates and shows at 2 θ angles are 20～25 °
An existing disperse peak, illustrates made aeroge for amorphous material.Density and N2Absorption detection shows, made prepared silicon dioxide airsetting
The density of glue is 0.08g/cm3, BET surface area 875m2/g；Main distribution 20nm in aperture～80nm, average pore size 40nm.
Embodiment 6
The method that the present embodiment prepares aerosil with quartz tail sand as raw material is comprised the following steps：
Step one, quartz tail sand is sequentially passed through washing, drying, grinding and cross 325 mesh sieves process, obtain quartz tail sand powder
End, then by the quartz tail sand powder and powdered sodium carbonate 0.9: 1 ground and mixed 30min in mass ratio, obtains mixed-powder,
Afterwards the mixed-powder being placed in Muffle furnace, 60min is calcined under conditions of temperature is 1300 DEG C, obtain calcined product；
Step 2, will calcined product described in step one grind after cross 200 mesh sieves, extracting screen underflow, then by described sieve under
Thing is added to stirring and dissolving 60min in the hot water that temperature is 90 DEG C, obtains waterglass after filtration；The matter of the siftage and hot water
Amount is than being 1: 4；
The pH value of waterglass described in step 2 is adjusted to 3 by step 3, the hydrochloric acid using concentration for 0.5mol/L, standing
Obtain hydrogel after 20min, then by the hydrogel temperature be 40 DEG C under conditions of aging 5d, obtain aging after water-setting
Glue；
Step 4, be filtered to remove aging described in step 3 after hydrogel in Free water, then adopt dehydrated alcohol
Enter line replacement to residuing in hydrogel surface and the absorption water in hole, obtain alcogel；The number of times of the displacement is 6 times, per
Used by secondary displacement, the volume of dehydrated alcohol is 3 times of hydrogel volume, and the temperature of displacement is 50 DEG C every time, each displacement
Time is 3h；As cleaning mixture, the hydrogel after aging is washed using deionized water during filtration, described wash
The number of times that washs is 4 times, and the volume of washing institute deionized water is 2 times of hydrogel volume every time；
Alcogel described in step 5, the hexane solution soaking step four using trim,ethylchlorosilane, hydrophobic to carry out
The displacement of modified and normal hexane, obtains the alkane gel of hydrophobically modified after washing；The number of times of the immersion is 5 times, soaks every time used
The volume of the hexane solution of trim,ethylchlorosilane is 4 times of alcogel volume, and the temperature for soaking displacement every time is 20 DEG C,
The time that soaks every time is 5h；The weight/mass percentage composition of trim,ethylchlorosilane in the hexane solution of the trim,ethylchlorosilane
For 8%；The cleaning mixture that the washing is adopted is normal hexane, and the number of times of the washing is 4 times, every time the body of washing normal hexane used
Product is 2 times of the volume of gel；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out
Gradient dried, obtains aerosil；The temperature that during the gradient dried, each stage dries is successively
For 50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time that each stage dries is 5h.
To the test characterization result of the aerosil that the present embodiment is prepared with quartz tail sand as raw material it is：Infrared light
Spectrogram shows, in 1110cm-1、811cm-1、465cm-1The strong peak at place is the characteristic absorption of Si-O-Si, and prepared dioxy is described
SiClx Aerogel bodies are Si-O-Si network skeleton structure；In 3437cm-1And 1645cm-1The pole weak peak at place is the feature of H-OH
Absorb, the absorption aqueouss very little of aeroge is described；1253cm-1、845cm-1、754cm-1The strong peak at place is Si-C characteristic absorption,
2937cm-1、1457cm-1、968cm-1Locate as-CH3Characteristic absorption, illustrate that aeroge surface has substantial amounts of-CH3, and
957cm-1The Si-OH characteristic absorption at place is very weak, illustrates-OH the overwhelming majority in aeroge by-Si (CH3)3Replace.For water
Contact angle reach 112 °, show that hydrophobicity is preferable.XRD tests made aeroge collection of illustrative plates and shows at 2 θ angles are 20～25 °
An existing disperse peak, illustrates made aeroge for amorphous material.Density and N2Absorption detection shows, made prepared silicon dioxide airsetting
The density of glue is 0.07g/cm3, BET surface area 806m2/g；Main distribution 5nm in aperture～70nm, average pore size 25nm.
The above, be only presently preferred embodiments of the present invention, not the present invention imposed any restrictions.Every according to invention skill
Any simple modification, change and equivalence changes that art is substantially made to above example, all still fall within technical solution of the present invention
Protection domain in.
Claims (10)
1. a kind of method that aerosil is prepared as raw material with quartz tail sand, it is characterised in that the method includes following
Step：
Step one, quartz tail sand is sequentially passed through washing, process of drying, grind and sieve, quartz tail sand powder is obtained, then will
The quartz tail sand powder and powdered sodium carbonate (0.8～1.6) in mass ratio: 1 ground and mixed, mixed-powder is obtained, afterwards will
The mixed-powder is placed in Muffle furnace and calcines, and obtains calcined product；
Step 2, will calcined product described in step one grind after sieve, extracting screen underflow, then the siftage is added to heat
In water, stirring and dissolving 60min～150min, filters to take filtrate afterwards, obtains waterglass；The mass ratio of the siftage and hot water
For 1: (3～5)；
Step 3, using hydrochloric acid, the pH value of waterglass described in step 2 is adjusted to 3～5, obtains after standing 20min～50min
Hydrogel, then by the hydrogel temperature be 40 DEG C～60 DEG C under conditions of aging 3d～5d, obtain aging after water-setting
Glue；
Step 4, the hydrogel after aging described in step 3 is filtered, so that the Free water in hydrogel is removed, then adopt
Enter line replacement with dehydrated alcohol to residuing in hydrogel surface and the absorption water in hole, obtain alcogel；
Step 5, alcogel described in step 4 is soaked in the hexane solution of trim,ethylchlorosilane, to carry out hydrophobic changing
Property and displacement of the normal hexane to ethanol, obtain the alkane gel of hydrophobically modified after washing；
Step 6, by the alkane gel of hydrophobically modified described in step 5 in drying at room temperature environment air-dry 24h, then carry out gradient
Dried, obtains aerosil；In the gradient dried process, the temperature of each stage dried is followed successively by
50 DEG C, 70 DEG C, 100 DEG C and 120 DEG C, the time of each stage dried is 3h～5h.
2. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the time of ground and mixed described in step one is 30min.
3. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the temperature that calcines described in step one is 1100 DEG C～1400 DEG C, the time of the calcining is 60min～150min.
4. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the temperature of hot water described in step 2 is 60 DEG C～90 DEG C.
5. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the concentration of hydrochloric acid described in step 3 is 0.1mol/L～0.5mol/L.
6. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the number of times that replaces described in step 4 is 3～6 times, the volume of displacement dehydrated alcohol used is hydrogel volume every time
1～6 times, every time displacement is all carried out under conditions of temperature is 30 DEG C～50 DEG C, every time the time of displacement be 3h～5h.
7. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, as cleaning mixture, the hydrogel after aging is washed using deionized water during filtering described in step 4,
The number of times of the washing is 3～4 times, every time the volume of washing institute deionized water be aging after hydrogel volume 2～3
Times.
8. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the number of times for soaking described in step 5 is 3～5 times, soaks the body of the hexane solution of trim,ethylchlorosilane used every time
Product is 1～6 times of alcogel volume, and soaking every time is all carried out under conditions of temperature is 20 DEG C～40 DEG C, is soaked every time
Time is 3h～5h.
9. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
Be, in the hexane solution of trim,ethylchlorosilane described in step 5 the weight/mass percentage composition of trim,ethylchlorosilane be 6%～
10%.
10. a kind of method that aerosil is prepared as raw material with quartz tail sand according to claim 1, its feature
It is, the cleaning mixture for washing employing described in step 5 is normal hexane, the number of times of the washing is 3～5 times, and washing is used every time
The volume of normal hexane is 2～3 times of alcogel volume.
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| CN108658130A (en) * | 2018-07-18 | 2018-10-16 | 浙江工业大学 | A method of preparing iron oxide and aerosil simultaneously from iron tailings |
| CN109012517A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A method of compound silica-based aerogel is prepared by raw material of iron tailings |
| CN111948095A (en) * | 2020-07-22 | 2020-11-17 | 电子科技大学 | Method for testing density of PZT aerogel |
| CN113264533A (en) * | 2021-06-30 | 2021-08-17 | 同济大学 | Method for preparing nano silicon dioxide aerogel by using waste glass |
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