CN107723800A - The method of Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution - Google Patents
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution Download PDFInfo
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- CN107723800A CN107723800A CN201710983206.4A CN201710983206A CN107723800A CN 107723800 A CN107723800 A CN 107723800A CN 201710983206 A CN201710983206 A CN 201710983206A CN 107723800 A CN107723800 A CN 107723800A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
- C30B29/62—Whiskers or needles
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, belongs to technical field of mineral processing in a kind of inorganic salt solution.This method includes:Desulfurated plaster and chemical additives are dissolved in inorganic salt solution, stirred, are configured to slurry;Slurry is placed in microwave reactor, microwave reaction temperature:85~110 DEG C, the reaction time:0.5~2h, obtain reacted slurry;Wherein, the power of microwave reactor is 400~800W, and microwave frequency is 2450 ± 50MHz;By the slurry after microwave reaction, room temperature is naturally cooled to, is aged 2~6h, water washing is added to neutrality, vacuum filtration, obtains filtrate and solid product;Solid product is placed in microwave reactor, in 60~80 DEG C of dry 5~20min, obtains calcium sulfate crystal whiskers.This method has the advantages that synthesis rate is fast, synthesis temperature is low, product morphology size uniform and preparation process environmental protection.
Description
Technical field
The invention belongs to technical field of mineral processing, and in particular to Microwave-assisted synthesis calcium sulfate in a kind of inorganic salt solution
The method of whisker.
Background technology
Desulfurated plaster is a kind of industry byproduct that the industry flue gas desulfurization such as electric power, petrochemical industry, steel is formed.At present, take off
Sulphur gypsum is mainly used as preparing plasterboard, cement retarder, saline-alkali land soil conditioner, forms soot material, be recessed for mine
Fall into the recovery in area etc..In addition to these are directly applied, because the main component of desulfurated plaster is dihydrate gypsum, so can
With for preparing the calcium sulfate crystal whiskers of high added value.Compared with other inorganic fibers, calcium sulfate crystal whiskers have production cost
The advantages that low, nontoxic, high temperature resistant, high mechanical strength, and can apply to composite synthesis, friction material synthesis, building
The fields such as engineering, papermaking, environmental protection.
In recent years, there are many patents on preparing calcium sulfate crystal whiskers using desulfurated plaster, the method mainly used is water
Hot method, normal pressure salt solustion mehtod and cooling recrystallization method.One kind desulfurated plaster is provided in patent CN101994153A and is prepared and is changed
Property calcium sulfate crystal whiskers method, this method passes through sieving, slurrying, hydro-thermal reaction, whisker surface modified, dehydration, drying and other steps
Obtained wastewaters with modified calcium sulfate whiskers, 0.5~6 micron of wastewaters with modified calcium sulfate whiskers diameter prepared by hydro-thermal method, 30~300 microns of length,
Draw ratio 15~115.A kind of technique that calcium sulfate crystal whiskers are prepared by desulfurated plaster is provided in patent CN102605430A, should
Technique by feeding, ball milling, configuration slurry plus medium crystallization agent, hydro-thermal reaction (reaction temperature be 110~150 DEG C), dehydrate
Step prepares calcium sulfate crystal whiskers, and the quality that the technique prepares calcium sulfate crystal whiskers is higher, a diameter of 1~3 μm, and draw ratio is
100~150, and calcium sulfate crystal whiskers diameter distribution with draw ratio change it is smaller, whisker surface crystallization is good.In patent
A kind of method that hemihydrate calcium sulfate crystal whisker is prepared using steel plant's desulfurated plaster as raw material, this method are provided in CN104451856A
Sulfuric acid removal of impurities is added in desulfurated plaster by elder generation, high-purity half-H 2 O calcium sulphate that Hydrothermal Synthesiss, drying and other steps are prepared it is brilliant
Must, the average diameter of the high-purity hemihydrate calcium sulfate crystal whisker is about 3 μm, and average length is about 150 μm, and average aspect ratio is about
50.In patent CN101550602, by the way that desulfurated plaster, water and medium crystallization agent are sufficiently mixed, prepared using normal pressure salt solustion mehtod
Go out a diameter of 1~10 μm, length is 140~60 μm of calcium sulfate crystal whiskers.In patent CN103074667A, it is by main component
Stirring, heating in the raw material input sulfuric acid solution of calcium sulfate, the suspension cooling recrystallization after dissolving is prepared into calcium sulfate crystal whiskers.
In a word, forefathers have carried out a few thing in terms of desulfurated plaster prepares calcium sulfate crystal whiskers, but go back the existing time
Long, the problems such as synthesis temperature is higher, product appearance size is uneven and building-up process causes environmental pollution.It is therefore proposed that one
Kind generated time is shorter, synthesis temperature is relatively low, product morphology size is more uniform and the method for environmentally friendly synthesis calcium sulfate crystal whiskers, should
Method has very high realistic meaning.
The content of the invention
The purpose of the present invention is to utilize the spy that microwave synthesising reacting time is short, synthesis temperature is low and inorganic salt solution is environmentally friendly
Point, overcome some problems present in prior art, there is provided Microwave-assisted synthesis calcium sulfate is brilliant in a kind of inorganic salt solution
The method of palpus.This method is to utilize microwave radiation technology, and desulfurated plaster Fast back-projection algorithm calcium sulfate crystal whiskers are utilized in inorganic salt solution.This
Invent and provide a kind of new method to prepare calcium sulfate crystal whiskers, with synthesis rate is fast, synthesis temperature is low, product morphology size is equal
The advantages that uniform preparation process environmental protection.
The method for realizing Microwave-assisted synthesis calcium sulfate crystal whiskers in a kind of inorganic salt solution of the present invention, according to following steps
Carry out:
Step 1, desulfurated plaster and chemical additives are dissolved in inorganic salt solution, stirred, be configured to slurry;
Wherein, the mass concentration of described inorganic salt solution is 4~45g/mL, in mass ratio, desulfurated plaster:Inorganic salts=(0.5~
8):(5~40);In mass ratio, chemical additives:Desulfurated plaster=(1~10):100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:85~110 DEG C, the reaction time:0.5~2h,
Obtain reacted slurry;Wherein, the power of microwave reactor is 400~800W, and microwave frequency is 2450 ± 50MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 2~6h, adds water washing to neutrality, very
Sky filters, and obtains filtrate and solid product;
Solid product is placed in microwave reactor, in 60~80 DEG C of dry 5~20min, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers prepared by the present invention are hemihydrate calcium sulfate crystal whisker, and whisker length is 30~120 μm, and diameter of whiskers is
1~4 μm, draw ratio is 30~75.
In described step 1, described desulfurated plaster is desulfurized gesso of flue gas;
In described step 1, described inorganic salts are appointing in sodium chloride, ammonium chloride, ammonium sulfate, potassium chloride, calcium chloride
The one or more of mixing of meaning.
In described step 1, described chemical additives are dodecyl sodium sulfate, neopelex, lemon
Any one or a few mixing in acid or copper chloride.
In described step 1, described desulfurated plaster, its quality is butt desulfurated plaster quality.
In described step 1, described stirs, and its stir speed (S.S.) is 100~150r/min, and mixing time is preferably
20~50min.
In described step 3, the power of described microwave reactor is 400~800W, microwave frequency is 2450 ±
50MHz。
The present invention is a kind of method of Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution, compared with prior art,
The features of the present invention and beneficial effect are:
Carried out 1. reacting in inorganic salt solution, do not add the acid to there is environment to have pollution and etching apparatus, but take
Obtained preferable effect.
2. reaction employs Microwave-assisted synthesis method, compared with 130 DEG C or so of normal heating conditions requirement, this method is closed
It is low into temperature, and during Microwave-assisted synthesis in addition to " fuel factor ", also " non-thermal effect " be present.In sulfuric acid
During calcium dissolution of crystals-recrystallization, the progress of microwave catalysis reaction, reaction activity is reduced, changes chemical reaction
Pre-exponential factor, change kinetics.
3. (001) face unidirectional growth speed of the crystal along nucleus can be accelerated by adding chemical additives during the course of the reaction
Rate.
4. product drying is carried out in microwave reactor, rapid draing can be not only realized, and a part can be ensured
Convert incomplete Dihydrate gypsum whiskers and be fully converted to hemihydrate calcium sulfate crystal whisker.
Brief description of the drawings
Fig. 1 is the desulfurated plaster scanning electron microscopic picture used in the embodiment of the present invention;
Fig. 2 is the X ray diffracting spectrum of the desulfurated plaster used in the embodiment of the present invention;
Fig. 3 is the X ray diffracting spectrum of hemihydrate calcium sulfate crystal whisker prepared by the embodiment of the present invention 1;
Fig. 4 is hemihydrate calcium sulfate crystal whisker scanning electron microscope (SEM) photograph prepared by the embodiment of the present invention 1;
Fig. 5 is hemihydrate calcium sulfate crystal whisker scanning electron microscope (SEM) photograph prepared by the embodiment of the present invention 2;
Fig. 6 is hemihydrate calcium sulfate crystal whisker scanning electron microscope (SEM) photograph prepared by the embodiment of the present invention 3;
Fig. 7 is hemihydrate calcium sulfate crystal whisker scanning electron microscope (SEM) photograph prepared by the embodiment of the present invention 4.
Embodiment
With reference to embodiment, the present invention is described in further detail.
The desulfurated plaster that following examples use comes from power plant of Liaoning Province;
Desulfurated plaster used is tested and analyzed, its scanning electron microscopic picture is shown in Fig. 1;
The X ray diffracting spectrum of desulfurated plaster used is shown in Fig. 2, it can be seen that the desulfurated plaster used is main
Composition is calcium sulphate dihydrate.
In following examples, except specified otherwise, used chemical reagent is the pure grade reagents of analysis purchased in market;
The INSTRUMENT MODEL that SEM scannings use in following examples is Japanese Shimadzu SEM-SS550, the instrument of XRD spectrum use
DX -2000 of device model Japan.
Embodiment 1
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas and dodecyl sodium sulfate are dissolved in sodium-chloride water solution, using stir speed (S.S.) as
After 110r/min stirrings 20min, slurry is configured to;Wherein, the mass concentration of described sodium-chloride water solution is 16.6g/mL, is pressed
Mass ratio, desulfurized gesso of flue gas:Sodium chloride=1:10;In mass ratio, dodecyl sodium sulfate:Desulfurized gesso of flue gas=3:100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:100 DEG C, the reaction time:40min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 500W, microwave frequency 2450MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 3h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 500W, microwave frequency 2450MHz, in 60 DEG C
5min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and its X ray diffracting spectrum is shown in Fig. 3, is obtained from Fig. 3
2 θ are 14.70 °, 25.60 °, 29.56 ° and 31.76 ° and half-H 2 O calcium sulphate crystal characteristic peak occur, it was demonstrated that it is half-H 2 O calcium sulphate
Whisker, its scanning electron microscope (SEM) photograph are shown in Fig. 4, and whisker average length is 90 μm, and whisker average diameter is 3 μm, average aspect ratio 30.
Embodiment 2
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas and neopelex are dissolved in aqueous ammonium chloride solution, with stir speed (S.S.)
After stirring 30min for 120r/min, slurry is configured to;Wherein, the mass concentration of described aqueous ammonium chloride solution is 26g/mL, is pressed
Mass ratio, desulfurized gesso of flue gas:Ammonium chloride=4:25;In mass ratio, neopelex:Desulfurized gesso of flue gas=4:
100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:90 DEG C, the reaction time:50min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 800W, microwave frequency 2400MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 3h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 800W, microwave frequency 2400MHz, in 70 DEG C
8min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and its scanning electron microscope (SEM) photograph is shown in Fig. 5, and whisker average length is
98.3 μm, whisker average diameter is 2.4 μm, average aspect ratio 40.9.
Embodiment 3
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas and citric acid are dissolved in potassium chloride solution, using stir speed (S.S.) as 130r/min
After stirring 40min, slurry is configured to;Wherein, the mass concentration of described potassium chloride solution is 31.9g/mL, in mass ratio,
Desulfurized gesso of flue gas:Potassium chloride=1:6;In mass ratio, citric acid:Desulfurized gesso of flue gas=5:100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:85 DEG C, the reaction time:80min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 400W, microwave frequency 2460MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 5h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 400W, microwave frequency 2460MHz, in 80 DEG C
10min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and its scanning electron microscope (SEM) photograph is shown in Fig. 6, and whisker average length is
102.5 μm, whisker average diameter is 1.9 μm, average aspect ratio 53.9.
Embodiment 4
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas and copper chloride are dissolved in calcium chloride water, using stir speed (S.S.) as 150r/min
After stirring 50min, slurry is configured to;Wherein, the mass concentration of described calcium chloride water is 42.8g/mL, in mass ratio,
Desulfurized gesso of flue gas:Calcium chloride=7:40;In mass ratio, copper chloride:Desulfurized gesso of flue gas=6:100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:85 DEG C, the reaction time:100min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 400W, microwave frequency 2460MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 6h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 500W, microwave frequency 2500MHz, in 60 DEG C
13min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and its scanning electron microscope (SEM) photograph is shown in Fig. 7, and whisker average length is
120 μm, whisker average diameter is 1.7 μm, average aspect ratio 70.6.
Embodiment 5
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas and copper chloride are dissolved in ammonium chloride and ammonium sulfate solution, using stir speed (S.S.) as
After 150r/min stirrings 40min, slurry is configured to;Wherein, the mass concentration of described ammonium chloride and ammonium sulfate solution is
33.3g/mL, in mass ratio, desulfurized gesso of flue gas:Ammonium chloride:Ammonium sulfate=8:20:20;In mass ratio, copper chloride:Flue gas takes off
Sulphur gypsum=6:100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:85 DEG C, the reaction time:120min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 400W, microwave frequency 2460MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 2h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 500W, microwave frequency 2500MHz, in 80 DEG C
15min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and whisker average length is 120 μm, whisker average diameter
For 1.6 μm, average aspect ratio 75.
Embodiment 6
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas, citric acid and copper chloride are dissolved in aqueous ammonium chloride solution, using stir speed (S.S.) as
After 100r/min stirrings 50min, slurry is configured to;Wherein, the mass concentration of described aqueous ammonium chloride solution is 33.3g/mL, is pressed
Mass ratio, desulfurized gesso of flue gas:Ammonium chloride=1:10;In mass ratio, copper chloride:Citric acid:Desulfurized gesso of flue gas=5:5:
100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:110 DEG C, the reaction time:30min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 400W, microwave frequency 2460MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 5h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 500W, microwave frequency 2500MHz, in 80 DEG C
20min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and whisker average length is 113.6 μm, and whisker is averagely straight
Footpath is 1.7 μm, average aspect ratio 66.8.
Embodiment 7
The method of Microwave-assisted synthesis calcium sulfate crystal whiskers, is followed the steps below in a kind of inorganic salt solution:
Step 1, desulfurized gesso of flue gas, citric acid and neopelex are dissolved in sodium-chloride water solution, with
Stir speed (S.S.) is after 100r/min stirs 50min, to be configured to slurry;Wherein, the mass concentration of described sodium-chloride water solution is
4g/mL, in mass ratio, desulfurized gesso of flue gas:Sodium chloride=1:80;In mass ratio, neopelex:Citric acid:Cigarette
Desulfurization gypsum=5:5:100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:110 DEG C, the reaction time:30min, obtain anti-
Slurry after answering;Wherein, the power of microwave reactor is 400W, microwave frequency 2500MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 4h, adds water washing to neutrality, vacuum
Filter, obtain filtrate and solid product;
Solid product is placed in microwave reactor, using microwave power as 500W, microwave frequency 2500MHz, in 60 DEG C
20min is dried, obtains calcium sulfate crystal whiskers.
Calcium sulfate crystal whiskers manufactured in the present embodiment are tested and analyzed, and whisker average length is 30 μm, whisker average diameter
For 1 μm, average aspect ratio 30.
Claims (7)
1. a kind of method of Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution, it is characterised in that this method is according to following
Step is carried out:
Step 1, desulfurated plaster and chemical additives are dissolved in inorganic salt solution, stirred, be configured to slurry;Its
In, the mass concentration of described inorganic salt solution is 4~45g/mL, in mass ratio, desulfurated plaster:Inorganic salts=(0.5~
8):(5~40);In mass ratio, chemical additives:Desulfurated plaster=(1~10):100;
Step 2, slurry is placed in microwave reactor, microwave reaction temperature:85~110 DEG C, the reaction time:0.5~2h, obtain
Reacted slurry;Wherein, the power of microwave reactor is 400~800W, and microwave frequency is 2450 ± 50MHz;
Step 3, by the slurry after microwave reaction, room temperature is naturally cooled to, is aged 2~6h, water washing to neutrality, vacuum is added and takes out
Filter, obtains filtrate and solid product;
Solid product is placed in microwave reactor, in 60~80 DEG C of dry 5~20min, obtains calcium sulfate crystal whiskers.
2. the method for Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution as claimed in claim 1, it is characterised in that institute
The calcium sulfate crystal whiskers of preparation are hemihydrate calcium sulfate crystal whisker, and whisker length is 30~120 μm, and diameter of whiskers is 1~4 μm, draw ratio
For 30~75.
3. the method for Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution as claimed in claim 1, it is characterised in that institute
In the step 1 stated, described desulfurated plaster is desulfurized gesso of flue gas.
4. the method for Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution as claimed in claim 1, it is characterised in that institute
In the step 1 stated, described inorganic salts be sodium chloride, ammonium chloride, ammonium sulfate, potassium chloride, in calcium chloride any one or it is several
Kind mixing.
5. the method for Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution as claimed in claim 1, it is characterised in that institute
In the step 1 stated, described chemical additives are dodecyl sodium sulfate, neopelex, citric acid or copper chloride
In any one or a few mixing.
6. the method for Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution as claimed in claim 1, it is characterised in that institute
In the step 1 stated, described stirs, and its stir speed (S.S.) is 100~150r/min, and mixing time is 20~50min.
7. the method for Microwave-assisted synthesis calcium sulfate crystal whiskers in inorganic salt solution as claimed in claim 1, it is characterised in that institute
In the step 3 stated, the power of described microwave reactor is 400~800W, and microwave frequency is 2450 ± 50MHz.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102352535A (en) * | 2011-09-22 | 2012-02-15 | 东莞上海大学纳米技术研究院 | Method for preparing calcium sulfate crystal whiskers from desulfurized gypsum under normal pressure |
CN102605430A (en) * | 2012-04-17 | 2012-07-25 | 河南城建学院 | Process for preparing calcium sulfate crystal whisker by desulfurized gypsum as well as calcium sulfate crystal whisker |
CN102925956A (en) * | 2012-11-26 | 2013-02-13 | 武汉科技大学 | Method for preparing calcium sulfate hemihydrate whiskers by taking ardealite as main raw material |
CN104894650A (en) * | 2015-05-31 | 2015-09-09 | 四川理工学院 | Method for preparing calcium sulfate dihydrate whisker from mirabilite and calcium water |
CN106431032A (en) * | 2016-06-30 | 2017-02-22 | 华南理工大学 | Microwave preparation method of alpha-calcium sulfate hemihydrate |
-
2017
- 2017-10-20 CN CN201710983206.4A patent/CN107723800A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102352535A (en) * | 2011-09-22 | 2012-02-15 | 东莞上海大学纳米技术研究院 | Method for preparing calcium sulfate crystal whiskers from desulfurized gypsum under normal pressure |
CN102605430A (en) * | 2012-04-17 | 2012-07-25 | 河南城建学院 | Process for preparing calcium sulfate crystal whisker by desulfurized gypsum as well as calcium sulfate crystal whisker |
CN102925956A (en) * | 2012-11-26 | 2013-02-13 | 武汉科技大学 | Method for preparing calcium sulfate hemihydrate whiskers by taking ardealite as main raw material |
CN104894650A (en) * | 2015-05-31 | 2015-09-09 | 四川理工学院 | Method for preparing calcium sulfate dihydrate whisker from mirabilite and calcium water |
CN106431032A (en) * | 2016-06-30 | 2017-02-22 | 华南理工大学 | Microwave preparation method of alpha-calcium sulfate hemihydrate |
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