CN107254710A - A kind of preparation method of the calcium sulfate crystal whiskers of low unit weight - Google Patents
A kind of preparation method of the calcium sulfate crystal whiskers of low unit weight Download PDFInfo
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- CN107254710A CN107254710A CN201710571298.5A CN201710571298A CN107254710A CN 107254710 A CN107254710 A CN 107254710A CN 201710571298 A CN201710571298 A CN 201710571298A CN 107254710 A CN107254710 A CN 107254710A
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- calcium sulfate
- unit weight
- preparation
- sulfate crystal
- crystal whiskers
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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
- C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
-
- 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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
-
- 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
Abstract
The invention discloses a kind of preparation method of the calcium sulfate crystal whiskers of low unit weight.The inventive method is mainly：Prepare forerunner's liquid suspension that solid holdup is no more than 30%；Presoma suspension pH value is adjusted to 3~6.5, and adds activator, 20~60min of stir-activating under the conditions of 60~80 DEG C；Suspension after pre-activate is injected into reactor, template is added, and 0.5~8h is reacted at 130~250 DEG C, until conversion is complete；Suspension after the completion of hydro-thermal reaction is subjected to separation of solid and liquid, and solid product is washed with the hot water for being not less than 70 DEG C；Solid product after separation and washing is dried into 0.5~5h under the conditions of 60 200 DEG C, product is produced.The calcium sulfate crystal whiskers structure that the present invention makes is novel, with larger surfaces externally and internally product and relatively low unit weight, is had a good application prospect in carrier, filler or adsorption cleaning field；The preparation method proposed is simple and direct efficiently, and extensively, cost is relatively low for raw material.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of preparation method of the calcium sulfate crystal whiskers of low unit weight.
Background technology
Calcium sulfate crystal whiskers are a kind of fibrous environmental protection inorganic materials grown with single crystal form, with some strength,
Price is relatively low, is increasingly applied in enhancing composite and papermaking etc. field, also has potential in building, medicine and field of Environment Protection
Application value.
Existing substantial amounts of patent and scientific paper have been carried out in method to the preparation of calcium sulfate crystal whiskers, modification and application
Inquire into.The crystal whisker preparation method proposed mainly has several major classes such as hydro-thermal method, normal pressure acidization and salt solustion mehtod.To improve sulphur
The application effect of sour calcium pyroborate, it was also proposed that the method that a variety of surfaces are modified.Such as, document 1 (Qian Liying, Liu Wenbo, what North Sea
The Chinese papermaking journals of new method [J] of Methods of Chemical Fibers Modification by Coating Natural Polymers, 2006,21 (4)：107-110) use
Cladding process suppresses whisker dissolving, improves paper retention and intensity.Patent CN101994153A uses desulfurated plaster hydro-thermal reaction
Directly modified prepare can reduce the whisker of aquation fracture, strengthen its compatibility with high polymer material.Patent CN102219930A
Mixed using atoleine, aluminate coupling agent LS-821 ultrasonic vibrations, the method that room temperature hangs and dried at 85-95 DEG C,
Improve calcium sulfate crystal whiskers and rubber, the interface compatibility of plastics.Calcium sulfate crystal whiskers also be used to adsorb waste water and gas by modified
In the pollutant such as heavy metal, the modified solubility for helping to reduce calcium sulfate crystal whiskers and its surface of raising and pollutant it is affine
Property.
But, it has been disclosed that synthesis and method of modifying obtained by crystal whisker products be interior solid whisker, although chi
Very little and draw ratio controllable, but structure is single, and specific surface area is smaller, and unit weight is larger.Therefore, traditional whisker and its modified product
Application performance in terms of filler and purification is done is by a definite limitation, and unit weight is larger also influences its economy.To break through
The deficiency of application performance, it is necessary to be improved to the bulk structure of crystal whisker products.
Polysaccharide is the macromolecular compound being formed by connecting by more than 10 monosaccharide molecules by dehydrating condensation, its stereo molecule
Contain the functional groups such as abundant hydroxyl, amino, carboxyl on chain.Research shows that mineral crystal often has on the single-minded site of polysaccharide
Fabulous orientation, the regulation of crystal structure and oriented growth can be realized by the use of polysaccharide as template.
The content of the invention
It is an object of the invention to for traditional calcium sulfate crystal whiskers unit weight it is larger the problem of there is provided a kind of sulfuric acid of low unit weight
The preparation method of calcium pyroborate.The calcium sulfate crystal whiskers of special construction are specifically prepared using pre-activate and hydro-thermal method regulation and control, make its body
Mutually there is cavity, reduce unit weight and increase specific surface area, more preferable architecture basics are provided for its functionalized application.
The preparation method of the calcium sulfate crystal whiskers of the low unit weight of the present invention, including following steps in sequence：
(1) prepared by presoma：Prepare forerunner's liquid suspension that solid holdup is no more than 30%；
(2) pre-activate：Presoma suspension pH value obtained by step (1) is adjusted to 3~6.5, and adds mass concentration and is
0.01~2% activator, 20~60min of stir-activating under the conditions of 60~80 DEG C；
(3) hydro-thermal reaction：Suspension after step (2) pre-activate is injected into reactor, adds 0.1~20g/L's
Template, and 0.5~8h is reacted at 130~250 DEG C, until conversion is complete；
(4) product separation and washing：Suspension after the completion of hydro-thermal reaction is subjected to separation of solid and liquid, and solid product is used
The hot water for being not less than 70 DEG C is washed, and reaction solution and washings return system are recycled；
(5) dry：Solid product after step (4) is separated and washed dries 0.5~5h under the conditions of 60-200 DEG C, i.e.,
Obtain product；No aquatic products can also be obtained by continuing calcining.
Specifically, it is CaSO by main component that step (1) the presoma preparation, which is,4Raw mineral materials it is broken after grind
To 40 mesh standard sieves, and dry 0.5~2h under the conditions of 120~200 DEG C is crossed, then it is mixed to prepare with water.
Either, directly or indirectly it is made with the salt or inorganic mineral of the element containing Ca with sulfuric acid solution hybrid reaction.It is mixed
The concentration ratio for closing reactant is not limited, and can be tested and determined according to the conventional debugger of those skilled in the art, fully to react
Completely, three waste discharge is reduced to be advisable.
Either, with containing Ca2+And SO4 2-Two kinds of solution mixing systems of ion are obtained.The concentration of two kinds of solution is not limited, can basis
The conventional debugger experiment of those skilled in the art is determined, fully to react complete, is reduced three waste discharge and is advisable.
Either, the mineral salt with the element containing Ca is with containing SO2Or SO3Gas mixing reaction, and be passed through air or oxygen
It is made after oxidation.The concentration that each material participates in reaction is not limited, and can test true according to the conventional debugger of those skilled in the art
It is fixed, fully to react complete, reduce three waste discharge and be advisable.
Above-mentioned forerunner's liquid suspension need to control solid holdup to be no more than 30%.When with three industrial wastes (acid waste water, acid waste gas
With calcium based mineral waste residue) when preparing presoma one of through the above way for raw material, necessary removal step (such as water can be taken
Wash, pickling or flotation etc.) to obtain the product of higher degree.
Specifically, the activator in step (2) is water-soluble lithium salts, magnesium salts and its mixture；Activator is preferably chlorination
One or more of mixtures in lithium, magnesium chloride, magnesium nitrate and magnesium sulfate.
Specifically, the structure regulating template that step (3) is added is cetyl trimethylammonium bromide (CTAB) and many
The mixture of sugar, its quality proportioning is CTAB：Polysaccharide=1：(5~30)；Polysaccharide be preferably glucose, soluble starch, shell gather
One or more mixtures in sugar and its soluble derivative.
The present invention prepares the calcium sulfate with hollow structure by the Hydrothermal Template control technique for being adapted to produce in enormous quantities
Whisker, to improve it as the performance of carrier, filler or scavenging material and improving economy and create favorable conditions.The present invention is comprehensive
Activation and hydrothermal recrystallization method technology, and by the spatial chemistry complementary effect and the molecular recognition in specific interface of polysaccharide template
Effect, induction prepares the calcium sulfate crystal whiskers with novel hollow cavity structure, so as to greatly reduce its unit weight, improves its application
Energy and economy.
The product prepared according to the inventive method is half water with cavity structure or without aqueous phase calcium sulfate crystal whiskers, length
10~800 μm, the μ m of diameter 0.5~50.The closely knit calcium sulfate crystal whiskers prepared relative to conventional method, this band cavity
Whisker reduce 15%~40% unit weight, and there is provided more rich inner surface, be expected in carrier, filler or sorbing material
More preferable effect is obtained when being applied Deng field.This method have it is simple and direct efficiently, raw material extensively, be adapted to large-scale production the advantages of.
The inventive method can also be with the process collection such as industrial acidic wastewater or high-salt wastewater, flue gas desulfurization and chemical gypsum treatment of wastes produced
Into realizing the comprehensive utilization of resource.
Brief description of the drawings
Fig. 1 is the electron microscope image (SEM) of calcium sulfate crystal whiskers prepared by conventional hydrothermal method.
The SEM image for the calcium sulfate crystal whiskers with cavity structure that Fig. 2 is prepared for the present invention.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.Accompanying drawing constitutes one of specification
Point, it is used to explain the present invention together with following specific embodiment, is not intended to limit the invention.Equipment used in embodiment
For chemical industry and mining industry field common equipment.
Embodiment one：
Natural crystal is used for raw material.By Gypsum Mine is broken, ground 40 mesh sieve, 100g is taken in 140 DEG C of drying box
1h is dried, progress presoma preparation is then mixed with 600mL water.By the regulation of presoma slurry pH value 4 or so, and add quality
The lithium chloride of concentration 0.2%, is then placed on stirring in beaker, is warming up to 60 DEG C of progress pre-activate.Slurries are turned after 0.5h
Move up into pressure-resistant reactor, otal investment is 1.2g structure regulating template.Wherein, cetyl trimethylammonium bromide
(CTAB) it is 0.2g, glucose is 0.8g, and chitosan is 0.2g.Then raise temperature to take out after 140 DEG C of progress hydro-thermal reactions, 4h and take out
Filter, while being washed with boiling water 3 times, then the solid product after suction filtration and washing is positioned in 60 DEG C of baking oven until being completely dried
Obtain the crystal whisker products of the present invention.This crystal whisker products have cavity structure and relatively low unit weight, by it is appropriate it is modified can
As carrier, filler or sorbing material etc..
Embodiment two：
Industrial gypsum (such as desulfurated plaster, ardealite and fluorgypsum solid waste) is used for raw material.Industrial gypsum is fully ground
Grind and cross 60 mesh sieves, carry out necessary removal of impurities processing, such as wash, sort.20g is taken to dry 0.5h in 150 DEG C of drying box,
Then completion presoma is mixed with 500mL water to prepare.By the regulation of presoma slurry pH value 5 or so, and add into slurries matter
The magnesium chloride of concentration 0.8% is measured, is then placed in beaker, is warming up to 70 DEG C and carries out pre-activate while stirring.After 20 minutes
Slurries are transferred into pressure-resistant reactor, otal investment is 2g structure regulating template.Wherein, cetyl trimethyl bromine
Change ammonium (CTAB) 0.3g, soluble starch 1.2g, chitosan is 0.5g.Then raise temperature to after 150 DEG C of progress hydro-thermal reactions, 3.5h
Suction filtration is taken out, while being washed with boiling water 3 times, then the solid product after suction filtration and washing is positioned in 60 DEG C of baking oven until complete
White drying is the crystal whisker products for obtaining the present invention.This crystal whisker products have cavity structure and relatively low unit weight, by suitably changing
It can be used as carrier, filler or sorbing material etc. after property.Embodiment three：
The natural crystal for containing abundant calcium constituent using dolomite, lime stone or calcite etc. is raw material.By ore reduction, grind
Honed 40 mesh sieve.Take 100g miberal powders to be put into beaker, first add 200~300ml concentration for 5%~15% hydrochloric acid that mineral are molten
Solution, is filtered off after sediment, then toward the sulfuric acid solution that addition 100ml~300ml concentration is 5%~40% in filtrate, stirring mixing is anti-
Presoma preparation should be completed.Then by the regulation of presoma slurry pH value 3.5 or so, and the sulfuric acid of mass content 1.2% is added
Magnesium, is placed in beaker and is warming up to 60 DEG C and carries out pre-activate while stirring.Slurries are transferred into pressure-resistant reactor after 1h,
Otal investment is 10.2g structure regulating template, wherein, CTAB0.4g, glucose 4.8g, soluble starch 5.0g.Then
160 DEG C of progress hydro-thermal reactions are warming up to, suction filtration are taken out after 4h, while wash with boiling water 3 times, then the solid phase by suction filtration and after washing
Product is positioned in 80 DEG C of baking oven until being completely dried the crystal whisker products for obtaining the present invention.This crystal whisker products have cavity
Structure and relatively low unit weight, carrier, filler or sorbing material etc. are can be used as by suitably modified.
Example IV：
It is raw material using the solution of chloride containing calcium and sodium sulphate (or sulfuric acid).Respectively 250ml is taken to contain Ca respectively2+Ion and
SO4 2-The solution of ion is mixed in beaker, and whether complementation is properly added completely depending on two kinds of initial concentration solution differences and reaction
, contain Ca2+Ion and SO4 2-The solution (can also be replaced with sulfuric acid, calcium salt or lime) of ion, stirring hybrid reaction ensures calcium
The less residual of ion, completes presoma and prepares.By the regulation of presoma slurry pH value 6 or so, and add mass content 0.2%
Lithium chloride and 0.6% magnesium chloride, be placed in beaker and be warming up to 80 DEG C and carry out pre-activate while stirring.Will slurry after 0.5h
Liquid is transferred into pressure-resistant reactor, and otal investment is 6g structure regulating template, and wherein CTAB is 0.4g, and glucose is
5.2g, carboxymethyl chitosan is 0.4g.Suction filtration is taken out after then raising temperature to 180 DEG C of progress hydro-thermal reactions, 3h, while being washed with boiling water
Wash 3 times, then the solid product after suction filtration and washing is positioned in 70 DEG C of baking oven until being completely dried obtains the present invention's
Crystal whisker products.This crystal whisker products have cavity structure and relatively low unit weight, by it is appropriate it is modified can be used as carrier, filler or
Sorbing material etc..
Embodiment five：
It is that raw material carries out presoma preparation using flue gas desulfurization course and desulfurization slag, and and then produces low unit weight whisker.Often
The more economical based Wet Process Flue Gas of rule be with calcium carbonate or lime slurry as absorbent, by absorption tower with containing
SO2Exhaust gas contact reaction reach purification purpose.The liquid of the calcium sulfite accessory substance (desulfurization slag) produced to flue gas desulfurization course
In be passed through enough air oxidations completely, control solid holdup below 30%, complete presoma prepare.Take 500ml forerunner's somaplasm
Liquid, control ph adds the magnesium sulfate of mass content 1% 6.5, is warming up to 65 DEG C of stirring pre-activate 1h.Then by slurries
It is transferred into pressure-resistant reactor, otal investment is 8g structure regulating template.Wherein, CTAB0.5g, soluble starch
2.5g, chitosan 0.15g.Suction filtration is taken out after being warming up to 200 DEG C of progress hydro-thermal reactions, 3.5h, while washed with boiling water 3 times, then
Solid product after suction filtration and washing is positioned in 70 DEG C of baking oven until being completely dried, that is, the whisker for obtaining the present invention is produced
Product.This crystal whisker products have cavity structure and relatively low unit weight, and carrier, filler or adsorption material are can be used as by suitably modified
Material etc..
Product prepared by the above method is the half aqueous phase calcium sulfate crystal whiskers with cavity structure, can also pass through high temperature
Calcining is produced out without aqueous phase whisker.Product be 10~800 μm of length, diameter in 0.5~50 μ m, volume to weight ratio conventional densification
Whisker is low by 15%~40%, as shown in Figure 1 and Figure 2.
It is described above be only the present invention flexible embodiment in enumerate it is several, for the ordinary skill of the art
For personnel, on the basis of the principle of the invention, some modifications can also be made, these modifications also should be regarded as the protection model of the present invention
Enclose.Obviously, it is appropriate to adjust separate step of the invention, feed change form or committed step of the present invention is integrated into acid or contained
In salt waste water, acid waste gas handling process, the same product effect of the present invention can also be obtained.Understand the present invention innovation it
Behind place, it can be achieved with without paying creative work.Therefore, these change, adjustment is obviously also to fall the guarantor in the present invention
Within the scope of shield.
Claims (9)
1. a kind of preparation method of the calcium sulfate crystal whiskers of low unit weight, it is characterised in that including following steps in sequence：
(1) prepared by presoma：Prepare forerunner's liquid suspension that solid holdup is no more than 30%；
(2) pre-activate：Presoma suspension pH value obtained by step (1) is adjusted to 3~6.5, and it is 0.01 to add mass concentration
~2% activator, 20~60min of stir-activating under the conditions of 60~80 DEG C；
(3) hydro-thermal reaction：Suspension after step (2) pre-activate is injected into reactor, 0.1~20g/L structure is added
Template, and 0.5~8h is reacted at 130~250 DEG C, until conversion is complete；
(4) product separation and washing：Suspension after the completion of hydro-thermal reaction is subjected to separation of solid and liquid, and not low is used to solid product
Washed in 70 DEG C of hot water, reaction solution and washings return system are recycled；
(5) dry：Solid product after step (4) is separated and washed dries 0.5~5h under the conditions of 60-200 DEG C, produces production
Product；No aquatic products can also be obtained by continuing calcining.
2. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 1, it is characterised in that：Before step (1) is described
Driving body and preparing is, is CaSO by main component4Raw mineral materials it is broken after be ground to 40 mesh standard sieves, and in 120~200 DEG C
Under the conditions of dry 0.5~2h, be then mixed to prepare with water.
3. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 1, it is characterised in that：Before step (1) is described
Driving body and preparing is, is directly or indirectly made with the salt or inorganic mineral of the element containing Ca with sulfuric acid solution hybrid reaction.
4. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 1, it is characterised in that：Before step (1) is described
Driving body and preparing is, with containing Ca2+And SO4 2-Two kinds of solution mixing systems of ion are obtained.
5. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 1, it is characterised in that：Before step (1) is described
Driving body and preparing is that the mineral salt with the element containing Ca is with containing SO2Or SO3Gas mixing reaction, and be passed through air or oxygen oxidation
After be made.
6. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 1, it is characterised in that：Work in step (2)
Agent is water-soluble lithium salts, magnesium salts and its mixture.
7. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 6, it is characterised in that：Activator is chlorination
One or more of mixtures in lithium, magnesium chloride, magnesium nitrate and magnesium sulfate.
8. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 1, it is characterised in that：Step (3) is added
Structure regulating template be the mixture of cetyl trimethylammonium bromide (CTAB) and polysaccharide, its quality proportioning is CTAB：
Polysaccharide=1：(5~30).
9. the preparation method of the calcium sulfate crystal whiskers of low unit weight according to claim 8, it is characterised in that：Polysaccharide be glucose,
One or more mixtures in soluble starch, chitosan and its soluble derivative.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111809228A (en) * | 2020-07-20 | 2020-10-23 | 湘潭大学 | Preparation method of calcium sulfate mineral crystal fiber |
| CN113105116A (en) * | 2021-03-31 | 2021-07-13 | 广东欧文莱陶瓷有限公司 | Digital carved ceramic and preparation method thereof |
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|---|---|---|---|---|
| CN104846440A (en) * | 2015-05-29 | 2015-08-19 | 昆明冶金研究院 | Method for preparing high-purity calcium sulfate dihydrate crystal whisker by using metallurgic flue gas desulfurization gypsum recrystallization process |
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2017
- 2017-07-13 CN CN201710571298.5A patent/CN107254710B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104846440A (en) * | 2015-05-29 | 2015-08-19 | 昆明冶金研究院 | Method for preparing high-purity calcium sulfate dihydrate crystal whisker by using metallurgic flue gas desulfurization gypsum recrystallization process |
Non-Patent Citations (1)
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| 丁润梅: "硫酸钙晶须制备方法及其除汞性能研究", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111809228A (en) * | 2020-07-20 | 2020-10-23 | 湘潭大学 | Preparation method of calcium sulfate mineral crystal fiber |
| CN113105116A (en) * | 2021-03-31 | 2021-07-13 | 广东欧文莱陶瓷有限公司 | Digital carved ceramic and preparation method thereof |
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