CN106084891A - A kind of modified conch meal calcine technology - Google Patents

A kind of modified conch meal calcine technology Download PDF

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CN106084891A
CN106084891A CN201610397797.2A CN201610397797A CN106084891A CN 106084891 A CN106084891 A CN 106084891A CN 201610397797 A CN201610397797 A CN 201610397797A CN 106084891 A CN106084891 A CN 106084891A
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conch meal
nano
titanium dioxide
powder
temperature
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CN106084891B (en
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朱荣华
卿宁
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Guangdong Beiyouan New Material Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/02Compounds of alkaline earth metals or magnesium
    • C09C1/021Calcium carbonates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00Compounds of titanium
    • C01G23/04Oxides; Hydroxides
    • C01G23/047Titanium dioxide
    • C01G23/053Producing by wet processes, e.g. hydrolysing titanium salts
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/006Combinations of treatments provided for in groups C09C3/04 - C09C3/12
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/04Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/06Treatment with inorganic compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C3/00Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
    • C09C3/10Treatment with macromolecular organic compounds

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The invention discloses a kind of modified conch meal calcine technology, with Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide and phenolic resin mixed pressuring plate when shell first is heated to occurring microcellular structure by this technique, then common high-temperature calcination, the Nano titanium dioxide of trace and nano-scaled electric stone powder can be completely dispersed in the micron openings of shell fine powder, load effect is the best, by high-temperature calcination, Organic substance is decomposed completely simultaneously, whole preparation process and product, to environment and human body non-hazardous, meet national requirements for environmental protection.

Description

A kind of modified conch meal calcine technology
Technical field
The present invention relates to the preparation method of conch meal, particularly relate to the calcine technology of a kind of modified conch meal.
Background technology
In recent years, along with environmental consciousness constantly strengthens, people are to the requirement of the performance of interior wall coating and safety increasingly Height, traditional coating after being moistened, easy breed bacteria, produce come off, the phenomenon such as variable color, have a strong impact on service life and room Interior attractive in appearance, the most indoor contaminated air cannot be carried out purified treatment.
Conch meal is by making after high-temperature calcination, pulverizing by natural seashell.Its constituent be calcium carbonate, calcium oxide, The calcified materials such as calcium hydroxide, this has absorption, the effect decomposing (formaldehyde, benzene, ammonia) etc. and regulation air wet as cellular The functions such as degree, the conch meal simultaneously fired to including including escherichia coli, Salmonella, staphylococcus aureus etc. multiple carefully Bacterium has extremely strong antibacterial and bactericidal action, and has the function of anticorrosion, mildew-resistant.Adding conch meal in coating, that makes is interior Wall coating will have good absorption harmful gas and fungistatic effect.
Chinese invention patent CN103011682A discloses a kind of coating adding conch meal, the invention provides a kind of shellfish The method of modifying of shell powder: the preparation process at Nano titanium dioxide adds tourmaline powder and conch meal, makes nanoscale titanium dioxide Titanium particle and tourmaline powder can more preferably be supported in the micropore of conch meal, will not come off because of scouring, release that can be permanent Go out anion room air to be purified and sterilization processing.But Nano titanium dioxide particle and tourmaline powder exist in this patent Load effect on conch meal is the best, needs repeatedly to load in preparation process, and process is loaded down with trivial details, purifies and bactericidal effect still needs to be carried High.
Summary of the invention
The technical problem existed based on background technology, the present invention proposes a kind of modified conch meal calcine technology.
A kind of modified conch meal calcine technology, comprises the following steps:
A, the soak with hydrochloric acid of shell 0.1-0.2% is cleaned 1h, wash away the organic of shell surface and inorganic impurity, spend Ionized water puts into oven drying after cleaning;
B, shell is heated in Muffle furnace 700 DEG C, keeps temperature lasting 4-6h, calcined product is ground, mistake 80 Mesh sieve, obtains conch meal;
C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide are stirred 15-20min, stir After mixing uniformly, it is heated to 200 DEG C, adds phenolic resin, stir, send in die arrangement, set press time, temperature And pressure, suppress, obtain tabletting;
D, tabletting is put in Muffle furnace calcine, be brought rapidly up to 700 DEG C, then gradually heat up with the speed of 5 DEG C/min To 900 DEG C, and persistently calcine 60-90min;
E, temperature is risen to 1200 DEG C, continue 25-30min, after cooling, calcined product is ground, cross 200 mesh sieves, to obtain final product To modified shell fine powder.
Preferably, the particle diameter of described Nano titanium dioxide is 30-50nm, the particle diameter of described nano-scaled electric stone powder For 60-80nm.
Preferably, in described step C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide with The percentage by weight of phenolic resin is respectively as follows: 80-85%, 0.1-0.2%, 0.2-0.3%, 0.5-0.8%, 15-20%.
Preferably, the parameter of die arrangement is set as: thickness 3-5mm, press time 5-10min, temperature 200-300 DEG C, Pressure 35-40MPa.
Preferably, step D, E course of reaction in, be ceaselessly passed through by ventilation unit abundance air.
Preferably, the preparation method of described nano-scaled electric stone powder, comprise the following steps:
A, tourmaline is ground to powder, crosses 120 mesh sieves, extracting screen underflow, obtain tourmaline powder;
B, being dissolved in water by tourmaline powder, carry out ultrasonic disperse, 80 mesh filter screens filter and go the removal of impurity, then carry out wet method Grind, it is thus achieved that natural sedimentation after slurry, then by mechanical means sediment separate out, precipitate sends wet grinding link back to again Participate in grinding;
C, sedimentary slurry adds wetting agent removing, use ultrasonic disperse, and suspension filter pressing is obtained filter Cake;Use high-energy ball milling that filter cake is ground, accelerate precipitation by centrifugation, isolate extra-fine grinding precipitate, send back to Extra-fine grinding link participates in grinding again;Removing sedimentary extra-fine grinding slurry, obtain filter cake by filter pressing, dry acquisition is received Meter level tourmaline powder.
Preferably, the preparation method of described Nano titanium dioxide, comprise the following steps:
A, n-butyl alcohol is diluted butyl titanate dissolve obtain the titanium precursors solution that concentration is 0.1-0.25mol/L;
B, n-butyl alcohol, dodecylbenzene sodium sulfonate mixed solution are added in high-temperature pressurizing reactor, solution is heated to 120 DEG C, and boost to 6-8MPa from normal pressure, then enough titanium precursors solution is added drop-wise in solution, stirs 8-10 hour Carrying out condensation reaction, during reaction, temperature is gradually warming up to 200 DEG C from 120 DEG C;
C, by reaction gained solution centrifugal after use straight alcohol dispensing laundry, be dried in a vacuum, obtain titanium source, therein The rotating speed of centrifuge is 2000-3500rpm;
D, titanium source is calcined under the conditions of 350-950 DEG C 2-3 hour, then the product after calcining is cooled to room temperature, To Nano titanium dioxide.
Molybdenum bisuphide is important kollag, is particularly well-suited under High Temperature High Pressure.It is described as, and " senior solid moistens Lubricating oil king ".The solid powder that molybdenum bisuphide is changed molecular structure by natural molybdenum concntrate powder after chemical purification and makes.This product Darkish complexion slightly band silver gray, has metallic luster, and that touches has a soapy feeling, water insoluble.Product has good dispersion, inadherent excellent Point, can be added in various oils and fats, forms exhausted inadherent colloidal state, can increase lubricity and the extreme pressure property of oils and fats.Also fit For high temperature, high pressure, the machine work state of high rotating speed high load capacity, extension device life-span.
In the present invention, shell being heated in Muffle furnace 700 DEG C, keep temperature lasting 4-6h, shell starts to occur micro- Cavernous structure, hole is less, but owing to reaction continue for 4-6h, therefore hole spreads all over shell surface and inside.Shell after calcining is ground It is milled to the micron order conch meal of 80 mesh, by conch meal and Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide and phenolic aldehyde Mixed with resin, it is therefore an objective to Nano titanium dioxide, nano-scaled electric stone powder are sufficiently mixed with conch meal, molybdenum bisuphide is lubrication Agent, and phenolic resin is binding agent, the close slabbing of convenient compacting, then by tabletting from 700 DEG C, with the speed of 5 DEG C/min Being gradually heating to 900 DEG C, and persistently conch meal surface micron order macropore can be occurred by calcining 60-90min, calcium carbonate is thorough simultaneously The end, is decomposed into calcium oxide, and discharges great amount of carbon dioxide, makes conch meal surface have huge specific surface area, and its absorbability is big Big enhancing, can be completely fixed in Nano titanium dioxide and nano-scaled electric stone powder in micron openings, finally temperature is raised To 1200 DEG C, continue 25-30min, the Organic substances such as phenolic resin are decomposed completely.
Correlated response formula is (under conditions of oxygen abundance):
Organic substance=H2O+ carbohydrate+CO2(> 700 DEG C)
CaCO3=CaO+CO2(> 900 DEG C)
Organic substance=H2O+CO2(> 1200 DEG C).
The invention have benefit that:
With Nano titanium dioxide, nano-scaled electric stone powder, curing when 1, shell first be heated to occurring microcellular structure Molybdenum and phenolic resin mixed pressuring plate, then common high-temperature calcination, can be by the Nano titanium dioxide of trace and nano-scaled electric Stone powder is completely dispersed in the micron openings of shell fine powder, and load effect is the best, it is not necessary to repeatedly load, and uses the modification of the present invention The preparation method of shell fine powder can reach low cost, high efficiency effect, ring prepared by this modification shell fine powder of final utilization Friendly coating possesses good air cleaning, sterilization processing and negative ion releasing function.
2, the phenolic resin simultaneously added in the present invention is under conditions of being passed through large quantity of air, the most at high temperature becomes Steam and carbon dioxide, to environment and human body non-hazardous, and the modified shell fine powder prepared is without Organic substance, is inorganic Thing, whole preparation process and product, all to environment and human body non-hazardous, are the conch meal preparation methoies of a kind of health, environmental protection.
Detailed description of the invention
Embodiment 1:
A kind of modified conch meal calcine technology, comprises the following steps:
A, by shell with 0.15% soak with hydrochloric acid clean 1h, wash away the organic of shell surface and inorganic impurity, spend from Sub-water puts into oven drying after cleaning;
B, shell is heated in Muffle furnace 700 DEG C, keeps temperature lasting 5h, calcined product is ground, mistake 80 mesh Sieve, obtains conch meal;
C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide being stirred 18min, stirring is all After even, it be heated to 200 DEG C, add phenolic resin, stir, send in die arrangement, set press time, temperature and pressure Power, suppresses, and obtains tabletting;The parameter of die arrangement is set as: thickness 4mm, press time 8min, temperature 250 DEG C, pressure 35MPa。
D, tabletting is put in Muffle furnace calcine, be brought rapidly up to 700 DEG C, then gradually heat up with the speed of 5 DEG C/min To 900 DEG C, and persistently calcine 70min;
E, temperature is risen to 1200 DEG C, continue 25min, after cooling, calcined product is ground, cross 200 mesh sieves, i.e. obtain Modified shell fine powder.
Preferably, the particle diameter of described Nano titanium dioxide is 30-50nm, the particle diameter of described nano-scaled electric stone powder For 60-80nm.
In described step C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide and phenolic resin Percentage by weight be respectively as follows: 83%, 0.15%, 0.25%, 0.6%, 16%.
Step D, E course of reaction in, be ceaselessly passed through by ventilation unit abundance air.
The preparation method of described nano-scaled electric stone powder, comprises the following steps:
A, tourmaline is ground to powder, crosses 120 mesh sieves, extracting screen underflow, obtain tourmaline powder;
B, being dissolved in water by tourmaline powder, carry out ultrasonic disperse, 80 mesh filter screens filter and go the removal of impurity, then carry out wet method Grind, it is thus achieved that natural sedimentation after slurry, then by mechanical means sediment separate out, precipitate sends wet grinding link back to again Participate in grinding;
C, sedimentary slurry adds wetting agent removing, use ultrasonic disperse, and suspension filter pressing is obtained filter Cake;Use high-energy ball milling that filter cake is ground, accelerate precipitation by centrifugation, isolate extra-fine grinding precipitate, send back to Extra-fine grinding link participates in grinding again;Removing sedimentary extra-fine grinding slurry, obtain filter cake by filter pressing, dry acquisition is received Meter level tourmaline powder.
The preparation method of described Nano titanium dioxide, comprises the following steps:
A, n-butyl alcohol is diluted butyl titanate dissolve obtain the titanium precursors solution that concentration is 0.2mol/L;
B, n-butyl alcohol, dodecylbenzene sodium sulfonate mixed solution are added in high-temperature pressurizing reactor, solution is heated to 120 DEG C, and boost to 7MPa from normal pressure, then enough titanium precursors solution is added drop-wise in solution, stirs and carry out for 10 hours Condensation reaction, during reaction, temperature is gradually warming up to 200 DEG C from 120 DEG C;
C, by reaction gained solution centrifugal after use straight alcohol dispensing laundry, be dried in a vacuum, obtain titanium source, therein The rotating speed of centrifuge is 3000rpm;
D, titanium source is calcined under the conditions of 600 DEG C 2.5 hours, then the product after calcining is cooled to room temperature, is received Meter level titanium dioxide.
Embodiment 2:
A kind of modified conch meal calcine technology, comprises the following steps:
A, by shell with 0.1% soak with hydrochloric acid clean 1h, wash away the organic of shell surface and inorganic impurity, use deionization Water puts into oven drying after cleaning;
B, shell is heated in Muffle furnace 700 DEG C, keeps temperature lasting 4h, calcined product is ground, mistake 80 mesh Sieve, obtains conch meal;
C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide being stirred 20min, stirring is all After even, it be heated to 200 DEG C, add phenolic resin, stir, send in die arrangement, set press time, temperature and pressure Power, suppresses, and obtains tabletting;The parameter of die arrangement is set as: thickness 5mm, press time 10min, temperature 300 DEG C, pressure Power 35MPa.
D, tabletting is put in Muffle furnace calcine, be brought rapidly up to 700 DEG C, then gradually heat up with the speed of 5 DEG C/min To 900 DEG C, and persistently calcine 70min;
E, temperature is risen to 1200 DEG C, continue 30min, after cooling, calcined product is ground, cross 200 mesh sieves, i.e. obtain Modified shell fine powder.
The particle diameter of described Nano titanium dioxide is 30-50nm, and the particle diameter of described nano-scaled electric stone powder is 60- 80nm。
In described step C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide and phenolic resin Percentage by weight be respectively as follows: 81%, 0.2%, 0.3%, 0.8%, 17.7%.
Step D, E course of reaction in, be ceaselessly passed through by ventilation unit abundance air.
The preparation method of described nano-scaled electric stone powder, comprises the following steps:
A, tourmaline is ground to powder, crosses 120 mesh sieves, extracting screen underflow, obtain tourmaline powder;
B, being dissolved in water by tourmaline powder, carry out ultrasonic disperse, 80 mesh filter screens filter and go the removal of impurity, then carry out wet method Grind, it is thus achieved that natural sedimentation after slurry, then by mechanical means sediment separate out, precipitate sends wet grinding link back to again Participate in grinding;
C, sedimentary slurry adds wetting agent removing, use ultrasonic disperse, and suspension filter pressing is obtained filter Cake;Use high-energy ball milling that filter cake is ground, accelerate precipitation by centrifugation, isolate extra-fine grinding precipitate, send back to Extra-fine grinding link participates in grinding again;Removing sedimentary extra-fine grinding slurry, obtain filter cake by filter pressing, dry acquisition is received Meter level tourmaline powder.
The preparation method of described Nano titanium dioxide, comprises the following steps:
A, n-butyl alcohol is diluted butyl titanate dissolve obtain the titanium precursors solution that concentration is 0.1mol/L;
B, n-butyl alcohol, dodecylbenzene sodium sulfonate mixed solution are added in high-temperature pressurizing reactor, solution is heated to 120 DEG C, and boost to 8MPa from normal pressure, then enough titanium precursors solution is added drop-wise in solution, stirs and contract for 8 hours Closing reaction, during reaction, temperature is gradually warming up to 200 DEG C from 120 DEG C;
C, by reaction gained solution centrifugal after use straight alcohol dispensing laundry, be dried in a vacuum, obtain titanium source, therein The rotating speed of centrifuge is 2000rpm;
D, titanium source is calcined under the conditions of 550 DEG C 3 hours, then the product after calcining is cooled to room temperature, obtains nanometer Grade titanium dioxide.
Embodiment 3
A kind of modified conch meal calcine technology, comprises the following steps:
A, by shell with 0.1% soak with hydrochloric acid clean 1h, wash away the organic of shell surface and inorganic impurity, use deionization Water puts into oven drying after cleaning;
B, shell is heated in Muffle furnace 700 DEG C, keeps temperature lasting 4h, calcined product is ground, mistake 80 mesh Sieve, obtains conch meal;
C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide being stirred 15min, stirring is all After even, it be heated to 200 DEG C, add phenolic resin, stir, send in die arrangement, set press time, temperature and pressure Power, suppresses, and obtains tabletting;The parameter of die arrangement is set as: thickness 3mm, press time 5min, temperature 200 DEG C, pressure 40MPa。
D, tabletting is put in Muffle furnace calcine, be brought rapidly up to 700 DEG C, then gradually heat up with the speed of 5 DEG C/min To 900 DEG C, and persistently calcine 70min;
E, temperature is risen to 1200 DEG C, continue 30min, after cooling, calcined product is ground, cross 200 mesh sieves, i.e. obtain Modified shell fine powder.
The particle diameter of described Nano titanium dioxide is 30-50nm, and the particle diameter of described nano-scaled electric stone powder is 60- 80nm。
In described step C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide and phenolic resin Percentage by weight be respectively as follows: 80%, 0.1%, 0.3%, 0.6%, 19%.
Step D, E course of reaction in, be ceaselessly passed through by ventilation unit abundance air.
The preparation method of described nano-scaled electric stone powder, comprises the following steps:
A, tourmaline is ground to powder, crosses 120 mesh sieves, extracting screen underflow, obtain tourmaline powder;
B, being dissolved in water by tourmaline powder, carry out ultrasonic disperse, 80 mesh filter screens filter and go the removal of impurity, then carry out wet method Grind, it is thus achieved that natural sedimentation after slurry, then by mechanical means sediment separate out, precipitate sends wet grinding link back to again Participate in grinding;
C, sedimentary slurry adds wetting agent removing, use ultrasonic disperse, and suspension filter pressing is obtained filter Cake;Use high-energy ball milling that filter cake is ground, accelerate precipitation by centrifugation, isolate extra-fine grinding precipitate, send back to Extra-fine grinding link participates in grinding again;Removing sedimentary extra-fine grinding slurry, obtain filter cake by filter pressing, dry acquisition is received Meter level tourmaline powder.
The preparation method of described Nano titanium dioxide, comprises the following steps:
A, n-butyl alcohol is diluted butyl titanate dissolve obtain the titanium precursors solution that concentration is 0.25mol/L;
B, n-butyl alcohol, dodecylbenzene sodium sulfonate mixed solution are added in high-temperature pressurizing reactor, solution is heated to 120 DEG C, and boost to 6MPa from normal pressure, then enough titanium precursors solution is added drop-wise in solution, stirs and contract for 9 hours Closing reaction, during reaction, temperature is gradually warming up to 200 DEG C from 120 DEG C;
C, by reaction gained solution centrifugal after use straight alcohol dispensing laundry, be dried in a vacuum, obtain titanium source, therein The rotating speed of centrifuge is 3500rpm;
D, titanium source is calcined under the conditions of 700 DEG C 3 hours, then the product after calcining is cooled to room temperature, obtains nanometer Grade titanium dioxide.
Hereinafter the partial parameters in technique is made a concrete analysis of:
Embodiment 4
Being adjusted by the particle diameter of the Nano titanium dioxide in embodiment 1, other technological parameters prepared are constant, with can Redispersibility latex powder is film forming matter, and the coating obtained carries out steel plate film, and thickness is 5mm, tests:
Knowable to above test data, the particle diameter of Nano titanium dioxide is the least, and the fungistatic effect of film is the best, but particle diameter When below 50nm, particle diameter reduces the least on the impact of bacteriostasis rate, therefore in order to reduce cost, the present invention selects 30-50nm particle diameter Nano titanium dioxide.
Embodiment 5
Being adjusted by the particle diameter of the nano-scaled electric stone powder in embodiment 1, other technological parameters prepared are constant, with can Redispersibility latex powder is film forming matter, and the coating obtained is carried out steel plate film, and thickness is 5mm, tests:
Knowable to above test data, the particle diameter of nano-tourmaline powder is the least, and the anion releasing effect of film is the best, but Particle diameter is when below 100nm, and particle diameter reduces the least on the impact of anion burst size, therefore in order to reduce cost, the present invention selects The nano-scaled electric stone powder of 60-80nm particle diameter.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto, Any those familiar with the art is in the technical scope of the present invention, according to technical scheme and invention thereof Conceive equivalent or change in addition, all should contain within protection scope of the present invention.

Claims (7)

1. a modified conch meal calcine technology, it is characterised in that comprise the following steps:
A, the soak with hydrochloric acid of shell 0.1-0.2% is cleaned 1h, wash away the organic of shell surface and inorganic impurity, use deionization Water puts into oven drying after cleaning;
B, shell is heated in Muffle furnace 700 DEG C, keeps temperature lasting 4-6h, calcined product is ground, mistake 80 mesh sieves, Obtain conch meal;
C, conch meal, Nano titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide being stirred 15-20min, stirring is all After even, it be heated to 200 DEG C, add phenolic resin, stir, send in die arrangement, set press time, temperature and pressure Power, suppresses, and obtains tabletting;
D, tabletting is put in Muffle furnace calcine, be brought rapidly up to 700 DEG C, be then gradually heating to 900 with the speed of 5 DEG C/min DEG C, and persistently calcine 60-90min;
E, temperature is risen to 1200 DEG C, continue 25-30min, after cooling, calcined product is ground, cross 200 mesh sieves, i.e. changed Property shell fine powder.
2. modified conch meal calcine technology as claimed in claim 1, it is characterised in that the grain of described Nano titanium dioxide Footpath is 30-50nm, and the particle diameter of described nano-scaled electric stone powder is 60-80nm.
3. conch meal calcine technology as claimed in claim 1 modified, it is characterised in that in described step C, conch meal, receives Meter level titanium dioxide, nano-scaled electric stone powder, molybdenum bisuphide are respectively as follows: 80-85%, 0.1-with the percentage by weight of phenolic resin 0.2%、0.2-0.3%、0.5-0.8%、15-20%。
4. modified conch meal calcine technology as claimed in claim 1, it is characterised in that the parameter of die arrangement is set as: thick Degree 3-5mm, press time 5-10min, temperature 200-300 DEG C, pressure 35-40MPa.
5. conch meal calcine technology as claimed in claim 1 modified, it is characterised in that step D, E course of reaction in, logical Cross ventilation unit and be ceaselessly passed through the air of abundance.
6. modified conch meal calcine technology as claimed in claim 1, it is characterised in that the system of described nano-scaled electric stone powder Preparation Method, comprises the following steps:
A, tourmaline is ground to powder, crosses 120 mesh sieves, extracting screen underflow, obtain tourmaline powder;
B, being dissolved in water by tourmaline powder, carry out ultrasonic disperse, 80 mesh filter screens filter and go the removal of impurity, then carry out wet method and grind Mill, it is thus achieved that natural sedimentation after slurry, then by mechanical means sediment separate out, precipitate is sent wet grinding link back to and is again joined With grinding;
C, sedimentary slurry adds wetting agent removing, use ultrasonic disperse, and suspension filter pressing is obtained filter cake;Adopt With high-energy ball milling, filter cake is ground, accelerates precipitation by centrifugation, isolate extra-fine grinding precipitate, send ultra-fine grinding back to Bull ring joint participates in grinding again;Remove sedimentary extra-fine grinding slurry, obtain filter cake by filter pressing, be dried and obtain nanoscale electricity Gas stone powder.
7. modified conch meal calcine technology as claimed in claim 1, it is characterised in that the system of described Nano titanium dioxide Preparation Method, comprises the following steps:
A, n-butyl alcohol is diluted butyl titanate dissolve obtain the titanium precursors solution that concentration is 0.1-0.25mol/L;
B, n-butyl alcohol, dodecylbenzene sodium sulfonate mixed solution are added in high-temperature pressurizing reactor, solution is heated to 120 DEG C, and boost to 6-8MPa from normal pressure, then enough titanium precursors solution is added drop-wise in solution, stirs 8-10 hour and carry out Condensation reaction, during reaction, temperature is gradually warming up to 200 DEG C from 120 DEG C;
C, after the solution centrifugal of reaction gained, use straight alcohol dispensing laundry, be dried in a vacuum, obtain titanium source, therein be centrifuged The rotating speed of machine is 2000-3500rpm;
D, titanium source is calcined under the conditions of 350-950 DEG C 2-3 hour, then the product after calcining is cooled to room temperature, is received Meter level titanium dioxide.
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CN107446497A (en) * 2017-08-01 2017-12-08 界首市宏利塑料有限公司 The barrier coating that a kind of plastics spoon uses when making
CN109894072A (en) * 2017-12-07 2019-06-18 秦皇岛贝壳森林环保科技有限公司 A kind of marine ecology nanometer conch meal and its method for being used to prepare conch meal base material for air purification
CN108246091A (en) * 2018-01-30 2018-07-06 广东汇雄实业投资有限公司 A kind of water soluble negative ion oyster shell whiting and its manufacture craft
CN108822579A (en) * 2018-07-04 2018-11-16 山东交通学院 A kind of modification shell powder preparation method with good dispersion
CN109045956A (en) * 2018-08-07 2018-12-21 赵文辉 A kind of vaccary deodorizing disinfectant and preparation method thereof
CN110893020A (en) * 2019-12-20 2020-03-20 湖州织里瑞茜服饰有限公司 Preparation method of low-cost nourishing type child underwear fabric
CN111825394A (en) * 2020-07-23 2020-10-27 广州市广丰混凝土有限公司 Anti-crack concrete
CN114605857A (en) * 2022-05-13 2022-06-10 佛山市顺德区温宝科技有限公司 Healthy and safe inorganic coating for building interior wall

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Denomination of invention: A calcination process of modified shell powder

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