CN106565269A - Method for preparing calcium sulfate whisker-silicon dioxide aerogel through normal-pressure drying - Google Patents
Method for preparing calcium sulfate whisker-silicon dioxide aerogel through normal-pressure drying Download PDFInfo
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- CN106565269A CN106565269A CN201610976952.6A CN201610976952A CN106565269A CN 106565269 A CN106565269 A CN 106565269A CN 201610976952 A CN201610976952 A CN 201610976952A CN 106565269 A CN106565269 A CN 106565269A
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- calcium sulfate
- aerosil
- crystal whiskers
- sulfate crystal
- precursor liquid
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
Abstract
The invention provides a method for preparing calcium sulfate whisker-silicon dioxide aerogel through normal-pressure drying. An aerogel precursor solution and a calcium sulfate whisker precursor solution are premixed and gelatinized, reaction conditions are controlled during normal-pressure drying, calcium sulfate whiskers are formed, and the calcium sulfate whiskers support and prevent collapse in the aerogel drying process. The method overcomes the defects that in a method for preparing silicon dioxide aerogel through a normal-pressure drying method, calcium sulfate inorganic fiber whiskers are adopted to serve as supporting materials to be directly added into gel, due to the fact that it is difficult to disperse the inorganic fiber whiskers into the gel uniformly, then a stable skeleton support of the aerogel cannot be formed, and the aerogel collapses in the drying process, the calcium sulfate whiskers and a silicon dioxide gel system are prepared in an in situ manner at the same time, the problem that the calcium sulfate whiskers are dispersed unevenly in the gel is avoided, moreover, integrity of the calcium sulfate whiskers is protected, the growth length of the calcium sulfate whiskers is controlled, and the prepared aerogel is high in heat-insulating property.
Description
Technical field
The present invention relates to field of inorganic nonmetallic material, and in particular to a kind of constant pressure and dry prepares calcium sulfate crystal whiskers-titanium dioxide
The method of silica aerogel.
Background technology
With going deep into for studying aerosil, research at present is concentrated on to low cost development.Aerogel material
Gradually it is applied to the fields such as building heat preservation, insulation of equipment, industrial pipeline insulation.Aeroge is cross-linked with each other structure by colloidal particle
Into with nanoporous spatial mesh structure, specific surface area is up to 500～1200m2·g-1, porosity up to 99.8%, its hole
Gap size is about 10～100nm, this nano-space structure, specific area porosity and its nanometer-size so as to have excellent
Different heat preservation and insulation.But because of its complicated process of preparation and technology content is very high, only carry in space flight and aviation, military project, medicine
Apply the high-end fields such as body.
The preparation of aerosil mainly adopts sol-gel process, is that one kind synthesizes under low temperature or temperate condition
The important method of inorganic material, is initially formed stable sol system, colloidal sol is aged or catalysis after be mutually polymerized between micelle, shape
Into the gel of three-dimensional net structure, the solvent for losing flowability is filled between gel network.Titanium dioxide is obtained by drying
Silica aerogel.However, in wet gel dry run, the solvent in wet gel stephanoporate framework passes through capillarity, osmosis
Wet gel surface is diffused into, gas-liquid interface is re-formed, and the capillary tension and aeroge aperture produced by solvent evaporation
Heterogeneity will cause skeleton to be macroscopically subject to bigger stress, cause framework shrinkage to ftracture and void collapse.Therefore, how to prevent
It is the key for preparing aeroge that aeroge does not cave in when being only dried.
Chinese invention patent application number 200410009902.8 discloses a kind of calcium silicates composite Nano hole superthermal insulation material
The preparation method of material.The invention is propped up with hollow secondary particle using what the xonotlite fiber of ultrafine diameter was formed as hard
Support bone frame and SiO2Aeroge is combined preparation method, first prepares what shaping was made up of ultrafine diameter eakleite crystal offspring
Block, shell and tiles product, while preparing SiO2Gel precursor, the eakleite that gel precursor pours into porous is produced
Product, then stand and enter gel and ageing process, and Jing autoclaves carry out supercritical drying, prepare calcium silicates composite Nano hole and surpass
Level heat-insulating material.Can effectively prevent from caving in using supercritical drying, but because Supercritical Drying Technology is high to equipment requirement, energy
Consumption is high, high cost, there is the factors such as security risk, causes aeroge cost high, hinders the application in building and industry
Development.Wish to produce inexpensive aeroge in batches using constant pressure and dry.
Chinese invention patent application number 201410655749.X discloses a kind of calcium sulfate crystal whiskers aerogel heat-proof composite wood
Material and preparation method thereof.First calcium sulfate crystal whiskers are carried out into surface to be modified, then by modified calcium sulfate crystal whiskers be added into through
In the tetraethyl orthosilicate mixed liquor of process, it is stirred continuously, obtains calcium sulfate crystal whiskers/SiO2Colloidal sol, through modified and immersion treatment,
Obtain calcium sulfate crystal whiskers/SiO2Aeroge.Although the invention is using cheap calcium sulfate crystal whiskers and inexpensive constant pressure and dry technique,
The high cost Supercritical Drying Technology for replacing aeroge generally to adopt in preparing, but, using calcium sulfate crystal whiskers as backing material
Add prevents during caving in when being dried due to being directly added into ca sulphate fibre dispersiveness defect in gel, causes to be difficult to and coagulates
Glue forms uniform network support.
Chinese invention patent application number 201410655832.7 discloses a kind of submicro inorganic whisker aerogel heat-proof and answers
Condensation material and preparation method thereof, the invention proposes a kind of submicro inorganic whisker aerogel heat-proof composite material and preparation method,
The invention is obtained Ludox with silicon alkoxide, alcoholic solvent as raw material first with hydrolysis, polycondensation, then utilizes at a certain temperature
Surfactant is carried out processing and obtains the submicro inorganic whisker well dispersed with Ludox to submicro inorganic whisker, is added
Ludox is combined, most after Jing is aging, one-step method surface modified and solvent displacement, submicro inorganic is prepared by constant pressure and dry
Whisker aerogel composite.It follows that the program is equally to employ addition inorganic crystal whisker, then disperseed, with silicon
Colloidal sol is combined, final to obtain submicro inorganic whisker aeroge, equally there is also submicro inorganic whisker dispersion problem
Cause the defect with gel-forming network support decreased effectiveness.
According to above-mentioned, during the method for aerosil is prepared currently with atmosphere pressure desiccation, using by calcium sulfate without
Machine fibrous crystal must be directly added in gel as backing material, due to it is difficult to effectively be dispersed in inorfil whisker solidifying
In glue, and then the stable skeletal support of aeroge cannot be formed, make aeroge subside when being dried, so, one kind is needed at present
Can either effectively dispersed inorfil whisker, the In-situ reaction preparation side of silica gel structure can be avoided damage to again
Method.
The content of the invention
For in the method that aerosil is prepared currently with atmosphere pressure desiccation, adopting calcium sulfate inorfil
Whisker is directly added in gel as backing material, due to being difficult that effectively inorfil whisker is dispersed in gel,
The stable skeletal support of aeroge cannot be further formed, makes aeroge there is subsiding when being dried.The present invention proposes a kind of normal pressure
The method that drying prepares calcium sulfate crystal whiskers-aerosil, aerogel precursor liquid and calcium sulfate crystal whiskers precursor liquid are premixed,
And gelation, control reaction condition in constant pressure and dry and form calcium sulfate crystal whiskers, caving in when supporting and prevent aeroge to be dried.
The present invention prepared calcium sulfate crystal whiskers and silica gel system are in situ simultaneously, it is to avoid calcium sulfate crystal whiskers disperse in gel
Uneven problem, and the integrality of calcium sulfate crystal whiskers is protected, control the growth length of calcium sulfate crystal whiskers, the gas of preparation
Gel heat-insulating property is more preferable.
The present invention provides a kind of method that constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, it is characterised in that
Preparation method is as follows：
（1）20-38.5 weight portion sea bittern slags, 40-50 weight portions milk of lime are mixed, is stirred, then pour 3-20 weight into
Part industrial waste acid, adjusts its pH and keeps to seething with excitement to 0-1.5 parts surfactants, heated solution between 3-4, is added
Fluid temperature is 60-70 DEG C, stands 0.1-5 hours, sulfuric acid calcium ion is completely dissolved in industrial waste acid, is then passed through
Filter, obtains calcium sulfate crystal whiskers precursor liquid；
（2）Silicon alkoxide is added in alcoholic solvent, the temperature of setting alcoholic solvent is 30-60 DEG C, and mixing speed is 100-500 rev/min
Under conditions of, water and industrial waste acid are sequentially added, its pH value is adjusted between 3-4, obtaining aerosil precursor liquid,
The silicon alkoxide, alcoholic solvent, water, the ratio of industrial waste acid are with molar ratio computing as 1:（5-40）:（2-10）:（1×10-5-5×10-5）；
（3）After the aerosil precursor liquid is stood into 0.1-24 hours in the case where temperature is for 30-80 DEG C, adjusting temperature is
60-70 DEG C, low whipping speed is described under conditions of 200-800 rev/min, to add drying control additive stirring 10-20 minutes
Silicon alkoxide, the mol ratio of drying control additive are 1:（0.25-0.5）；
（4）By step（3）Obtain the aerosil precursor liquid and step added with drying control additive（1）The sulphur for obtaining
Sour calcium pyroborate precursor liquid mixing, mixing speed is stirring 5-40 minutes under conditions of 300-500 rev/min, adds base catalysis
Agent, stirs 5-30 minutes, obtains calcium sulfate-aerosil complex sol, keeps the aerosil forerunner
The temperature of liquid and calcium sulfate crystal whiskers precursor liquid is 60-70 DEG C, is then cooled under conditions of 30-40 DEG C, stands 0.5-10 hours,
Calcium sulfate crystal whiskers-silica dioxide gel is obtained, then calcium sulfate crystal whiskers-silica dioxide gel is put in drying box, be in temperature
1-3 hours at 60-100 DEG C, obtain calcium sulfate crystal whiskers-aerosil.
Preferably, the sulfuric acid lean solution produced during the industrial waste acid is industrial production and mining, smelting.
Preferably, the surfactant is stearic acid, lauryl sodium sulfate, Tween-80, DBSA
At least one in sodium, aluminate coupling agent.
Preferably, the silicon alkoxide is tetraethyl orthosilicate, methyl silicate, silicic acid propyl ester, waterglass, diatomite, rice husk
At least one in ash.
Preferably, the alcoholic solvent is the combination of any one or more in methyl alcohol, ethanol, isopropanol, normal propyl alcohol.
Preferably, the base catalyst is at least one in ammoniacal liquor, NaOH, ammonium fluoride.
Preferably, the drying control additive is in formamide, acetamide, DMF, glycerine
Any one.
Preferably, step（4）The aerosil precursor liquid added with drying control additive is brilliant with calcium sulfate
Palpus precursor liquid is with mass ratio 100：（20-60）Mixing.
A kind of method that constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, compared with prior art, its protrusion
The characteristics of and excellent effect be：
1st, the present invention is using inexpensive constant pressure and dry technique, the high cost supercritical drying for replacing aeroge generally to adopt in preparing
Technology, significantly reduces the production cost of aerogel heat-insulating material, is capable of achieving the scale of calcium sulfate crystal whiskers aerogel composite
Change and streaming production, and it is simple to operate, it is suitable for related personnel's operation, through related training, it is easy to grasp.
2nd, the present invention is prepared calcium sulfate crystal whiskers and silica gel system are in situ simultaneously, it is to avoid calcium sulfate crystal whiskers
Disperse uneven problem in gel, and protect the integrality of calcium sulfate crystal whiskers, control the growth of calcium sulfate crystal whiskers
Length, the heat-insulating property of aeroge is more preferable.
3rd, using sea bittern slag and industrial waste acid as raw material, abundance is cheap, with obvious Jing for the present invention
Ji benefit.
4th, the whole production process cleaning of the present invention, environmental protection, the calcium sulfate crystal whiskers-aerosil of preparation is heat-insulated compound
Material is resistant to 1500 DEG C of high temperature.
Specific embodiment
Below by way of specific embodiment, the present invention is described in further detail, but this should not be interpreted as into the present invention
Scope be only limitted to Examples below.In the case of without departing from said method thought of the present invention, according to ordinary skill
Various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）20 weight portion sea bittern slags, 40 weight portion milk of limes are mixed, are stirred, then pour 10 weight portion industrial waste acids into,
Adjust its pH and keep fluid temperature to seething with excitement to 0.1 parts surfactant stearic acid, heated solution between 3-4, is added
For 60 DEG C, 0.1 hour is stood, sulfuric acid calcium ion is completely dissolved in industrial waste acid, then through filtering, obtain calcium sulfate brilliant
Must precursor liquid；Wherein, the sulfuric acid lean solution produced during industrial waste acid is industrial production and mining, smelting.
（2）Silicon alkoxide tetraethyl orthosilicate is added in alcoholic solvent methyl alcohol, the temperature of setting alcoholic solution methyl alcohol is 30 DEG C, stirring
Speed adjusts its pH value between 3-4 under conditions of 100 revs/min, to sequentially add water and industrial waste acid, obtains titanium dioxide
Silica aerogel precursor liquid, the silicon alkoxide, alcoholic solvent, deionized water, the ratio of industrial waste acid are with molar ratio computing as 1:5:2:1×
10-5；
（3）After aerosil precursor liquid is stood into 0.1 hour in the case where temperature is for 30 DEG C, it is 60 DEG C to adjust temperature, is being stirred
Speed is mixed under conditions of 200 revs/min, to add drying control additive formamide to stir 10 minutes, wherein, silicon alkoxide, drying
The mol ratio for controlling additive formamide is 1:0.25；
（4）By aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid with mass ratio 100：30 mix, and mixing speed is
Stir 5 minutes under conditions of 300 revs/min, add base catalyst ammoniacal liquor, stir 5 minutes, obtain calcium sulfate-silica
Aeroge complex sol, the temperature for keeping the aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid is 60 DEG C, so
After be cooled under conditions of 30 DEG C, stand 0.5 hour, obtain calcium sulfate crystal whiskers-silica dioxide gel, then calcium sulfate crystal whiskers-
Silica dioxide gel is put in drying box, is dried 3 hours in the case where temperature is for 100 DEG C, obtains calcium sulfate crystal whiskers-silica airsetting
Glue.
Calcium sulfate crystal whiskers-aerosil manufactured in the present embodiment preferably maintains the uniform hole of aeroge,
Jing performance tests, specific surface area is 680m2/ g or so, porosity up to 98%, pore size distribution range 12-16nm, average pore size
14nm。
Embodiment 2
（1）22 weight portion sea bittern slags, 42 weight portion milk of limes are mixed, are stirred, then pour 5 weight portion industrial waste acids into,
Adjust its pH and protect to seething with excitement to 1.1 parts by weight Surfactant SDSs, heated solution between 3-4, is added
Fluid temperature is held for 62 DEG C, 0.7 hour is stood, sulfuric acid calcium ion is completely dissolved in industrial waste acid, then through filtering, obtained
To calcium sulfate crystal whiskers precursor liquid, wherein, industrial waste acid is that the sulfuric acid produced during industrial production and mining, smelting gives up
Solution.
（2）Methyl silicate is added in alcoholic solvent ethanol, the temperature of setting alcoholic solution ethanol is 40 DEG C, and mixing speed is
Under conditions of 150 revs/min, deionized water and industrial waste acid are sequentially added, adjust its pH value between 3-4, obtain titanium dioxide
Silica aerogel precursor liquid, methyl silicate, ethanol, deionized water, the ratio of industrial waste acid are with molar ratio computing as 1:15:5:2×
10-5；
（3）After aerosil precursor liquid is stood into 0.5 hour in the case where temperature is for 40 DEG C, it is 62 DEG C to adjust temperature, is being stirred
Speed is mixed under conditions of 300 revs/min, to add drying control additive acetamide to stir 15 minutes, wherein, methyl silicate,
The mol ratio of drying control additive acetamide is 1:0.27；
（4）By aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid with mass ratio 100：20 mix, and mixing speed is
Stir 15 minutes under conditions of 350 revs/min, add base catalyst ammoniacal liquor, stir 15 minutes, obtain calcium sulfate-titanium dioxide
Silica aerogel complex sol, the temperature for keeping the aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid is 65 DEG C,
Then it is cooled under conditions of 32 DEG C, stands 0.7 hour, obtains calcium sulfate crystal whiskers-silica dioxide gel, then calcium sulfate is brilliant
Palpus-silica dioxide gel is put in drying box, is dried 1 hour in the case where temperature is for 80 DEG C, obtains calcium sulfate crystal whiskers-silica gas
Gel.
Embodiment 3
（1）25 weight portion sea bittern slags, 45 weight portion milk of limes are mixed, are stirred, then pour 10 weight portion industrial waste acids into,
Adjust its pH and protect to seething with excitement to 0.6 parts surfactant neopelex, heated solution between 3-4, is added
Fluid temperature is held for 65 DEG C, 0.8 hour is stood, sulfuric acid calcium ion is completely dissolved in industrial waste acid, then through filtering, obtained
To calcium sulfate crystal whiskers precursor liquid, wherein, industrial waste acid is that the sulfuric acid produced during industrial production and mining, smelting gives up
Solution.
（2）Silicic acid propyl ester is added in alcoholic solvent ethanol, the temperature of setting alcoholic solution isopropanol is 45 DEG C, and mixing speed is
Under conditions of 250 revs/min, deionized water and industrial waste acid are sequentially added, adjust its pH value between 3-4, obtain titanium dioxide
Silica aerogel precursor liquid, silicic acid propyl ester, isopropanol, distilled water, the ratio of industrial waste acid are with molar ratio computing as 1:28:9:2.8×
10-5；
（3）After aerosil precursor liquid is stood into 2 hours in the case where temperature is for 45 DEG C, it is 65 DEG C to adjust temperature, in stirring
Speed is under conditions of 500 revs/min, to add drying control additive glycerine to stir 17 minutes, wherein, it is methyl silicate, dry
The dry mol ratio for controlling additive acetamide is 1:0.3；
（4）By aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid with mass ratio 100：50 mix, and mixing speed is
Stir 25 minutes under conditions of 400 revs/min, add base catalyst NaOH, stir 20 minutes, obtain calcium sulfate-two
Silica aerogel complex sol, the temperature for keeping the aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid is 68
DEG C, then it is cooled under conditions of 35 DEG C, 2 hours are stood, calcium sulfate crystal whiskers-silica dioxide gel is obtained, then calcium sulfate is brilliant
Palpus-silica dioxide gel is put in drying box, is dried 2 hours in the case where temperature is for 90 DEG C, obtains calcium sulfate crystal whiskers-silica gas
Gel.
Embodiment 4
（1）30 weight portion sea bittern slags, 46 weight portion milk of limes are mixed, are stirred, then pour 12 weight portion industrial waste acids into,
Its pH is adjusted between 3-4, heated solution keeps fluid temperature to be 70 DEG C to seething with excitement, and stands 4 hours, fills sulfuric acid calcium ion
Divide and be dissolved in industrial waste acid, then through filtering, obtain calcium sulfate crystal whiskers precursor liquid, wherein, industrial waste acid is industrial production
With the sulfuric acid lean solution produced during mining, smelting.
（2）Tetraethyl orthosilicate and diatom earth mixtures are added the temperature that alcoholic solution isopropanol is arranged in alcoholic solvent ethanol
For 55 DEG C, mixing speed adjusts its pH value to 3-4 under conditions of 400 revs/min, to sequentially add distilled water and industrial waste acid
Between, obtain aerosil precursor liquid, positive silicic acid acetoacetic ester and diatom earth mixtures, isopropanol, distilled water, Industry Waste
The ratio of acid is with molar ratio computing as 1:40:10:5×10-5；
（3）After aerosil precursor liquid is stood into 12 hours in the case where temperature is for 65 DEG C, it is 68 DEG C to adjust temperature, in stirring
Speed is under conditions of 650 revs/min, to add drying control additive DMF to stir 18 minutes, wherein, positive silicon
Acetoacetic ester and diatom earth mixtures, the mol ratio of drying control additive N,N-dimethylformamide are 1:0.45；
（4）By aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid with mass ratio 100：20 mix, and mixing speed is
Stir 35 minutes under conditions of 500 revs/min, add base catalyst ammoniacal liquor and NaOH mixed liquor, stir 25 minutes, obtain
To calcium sulfate-aerosil complex sol, the aerosil precursor liquid and calcium sulfate crystal whiskers forerunner are kept
The temperature of liquid is 70 DEG C, is then cooled under conditions of 40 DEG C, stands 6 hours, obtains calcium sulfate crystal whiskers-silica dioxide gel,
Calcium sulfate crystal whiskers-silica dioxide gel is put in drying box again, is dried 3 hours in the case where temperature is for 100 DEG C, obtain calcium sulfate brilliant
Palpus-aerosil.
Embodiment 5
（1）38.5 weight portion sea bittern slags, 50 weight portion milk of limes are mixed, is stirred, then pour 20 weight portion Industry Wastes into
Acid, adjusts its pH between 3-4, and heated solution adds 1.5 mass of surface active agent tween -80 to seething with excitement, and keeps liquid
Temperature is 70 DEG C, stands 5 hours, sulfuric acid calcium ion is completely dissolved in industrial waste acid, then through filtering, obtains calcium sulfate
Whisker precursor liquid, wherein, industrial waste acid is the sulfuric acid lean solution produced during industrial production and mining, smelting.
（2）Rice hull ash and diatom earth mixtures are added in the mixed liquor of alcoholic solvent isopropanol and methyl alcohol, isopropanol is set
It it is 60 DEG C with the temperature of the mixed liquor of methyl alcohol, mixing speed is under conditions of 500 revs/min, to sequentially add pure water and industry
Spent acid, adjusts its pH value between 3-4, obtaining aerosil precursor liquid, rice hull ash and diatom earth mixtures, isopropyl
Alcohol, pure water, the ratio of industrial waste acid are with molar ratio computing as 1:40:10:5×10-5；
（3）After aerosil precursor liquid is stood into 24 hours in the case where temperature is for 75 DEG C, it is 70 DEG C to adjust temperature, in stirring
Speed is under conditions of 800 revs/min, to add drying control additive DMF to stir 20 minutes, wherein, rice husk
Ash and diatom earth mixtures, the mol ratio of drying control additive N,N-dimethylformamide are 1:0.5；
（4）By aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid with mass ratio 100：40 mix, and mixing speed is
Stir 40 minutes under conditions of 500 revs/min, add base catalyst ammoniacal liquor and ammonium fluoride mixed liquor, stir 25 minutes, obtain
Calcium sulfate-aerosil complex sol, keeps the aerosil precursor liquid and calcium sulfate crystal whiskers precursor liquid
Temperature be 70 DEG C, be then cooled under conditions of 40 DEG C, stand 10 hours, obtain calcium sulfate crystal whiskers-silica dioxide gel, then
Calcium sulfate crystal whiskers-silica dioxide gel is put in drying box, temperature be 70 DEG C at be dried 2 hours, obtain calcium sulfate crystal whiskers-
Aerosil.
Claims (8)
1. a kind of method that constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, it is characterised in that preparation method is as follows：
（1）20-38.5 weight portion sea bittern slags, 40-50 weight portions milk of lime are mixed, is stirred, then pour 3-20 weight into
Part industrial waste acid, adjusts its pH and keeps to seething with excitement to 0-1.5 parts surfactants, heated solution between 3-4, is added
Fluid temperature is 60-70 DEG C, stands 0.1-5 hours, sulfuric acid calcium ion is completely dissolved in industrial waste acid, is then passed through
Filter, obtains calcium sulfate crystal whiskers precursor liquid；
（2）Silicon alkoxide is added in alcoholic solvent, the temperature of setting alcoholic solvent is 30-60 DEG C, and mixing speed is 100-500 rev/min
Under conditions of, water and industrial waste acid are sequentially added, its pH value is adjusted between 3-4, obtaining aerosil precursor liquid,
The silicon alkoxide, alcoholic solvent, water, the ratio of industrial waste acid are with molar ratio computing as 1:（5-40）:（2-10）:（1×10-5-5×10-5）；
（3）After the aerosil precursor liquid is stood into 0.1-24 hours in the case where temperature is for 30-80 DEG C, adjusting temperature is
60-70 DEG C, low whipping speed is described under conditions of 200-800 rev/min, to add drying control additive stirring 10-20 minutes
Silicon alkoxide, the mol ratio of drying control additive are 1:（0.25-0.5）；
（4）By step（3）Obtain the aerosil precursor liquid and step added with drying control additive（1）The sulphur for obtaining
Sour calcium pyroborate precursor liquid mixing, mixing speed is stirring 5-40 minutes under conditions of 300-500 rev/min, adds base catalysis
Agent, stirs 5-30 minutes, obtains calcium sulfate-aerosil complex sol, keeps the aerosil forerunner
The temperature of liquid and calcium sulfate crystal whiskers precursor liquid is 60-70 DEG C, is then cooled under conditions of 30-40 DEG C, stands 0.5-10 hours,
Calcium sulfate crystal whiskers-silica dioxide gel is obtained, then calcium sulfate crystal whiskers-silica dioxide gel is put in drying box, be in temperature
1-3 hours at 60-100 DEG C, obtain calcium sulfate crystal whiskers-aerosil.
2. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：The industrial waste acid is the sulfuric acid lean solution produced during industrial production and mining, smelting.
3. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：The surfactant is stearic acid, lauryl sodium sulfate, Tween-80, neopelex, Aluminate idol
At least one in connection agent.
4. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：The silicon alkoxide be tetraethyl orthosilicate, methyl silicate, silicic acid propyl ester, waterglass, diatomite, rice hull ash at least
It is a kind of.
5. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：The alcoholic solvent is the combination of any one or more in methyl alcohol, ethanol, isopropanol, normal propyl alcohol.
6. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：The base catalyst is at least one in ammoniacal liquor, NaOH, ammonium fluoride.
7. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：The drying control additive is any one in formamide, acetamide, N,N-dimethylformamide, glycerine.
8. a kind of method that according to claim 1 constant pressure and dry prepares calcium sulfate crystal whiskers-aerosil, its feature
It is：Step（4）The aerosil precursor liquid added with drying control additive and calcium sulfate crystal whiskers precursor liquid with
Mass ratio 100：（20-60）Mixing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107964120A (en) * | 2017-12-27 | 2018-04-27 | 四川理工学院 | A kind of rubber function additive calcium sulfate crystal whiskers and the composite modified method of white carbon |
| CN108395197A (en) * | 2018-03-19 | 2018-08-14 | 河南城建学院 | A kind of wall heat insulation material of the compound desulfurated plaster whisker of aerosil |
| CN108455997A (en) * | 2018-01-29 | 2018-08-28 | 爱彼爱和新材料有限公司 | A kind of Al2O3-SiO2System high-performance nano cellular insulant and preparation method |
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| CN104446305A (en) * | 2014-11-17 | 2015-03-25 | 广州大学 | Calcium sulphate whisker aerogel heat-insulating composite material and preparation method thereof |
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| CN107964120A (en) * | 2017-12-27 | 2018-04-27 | 四川理工学院 | A kind of rubber function additive calcium sulfate crystal whiskers and the composite modified method of white carbon |
| CN108455997A (en) * | 2018-01-29 | 2018-08-28 | 爱彼爱和新材料有限公司 | A kind of Al2O3-SiO2System high-performance nano cellular insulant and preparation method |
| CN108395197A (en) * | 2018-03-19 | 2018-08-14 | 河南城建学院 | A kind of wall heat insulation material of the compound desulfurated plaster whisker of aerosil |
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Application publication date: 20170419 |