CN104264227A - Preparation method of gypsum crystal whisker - Google Patents
Preparation method of gypsum crystal whisker Download PDFInfo
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- CN104264227A CN104264227A CN201410481465.3A CN201410481465A CN104264227A CN 104264227 A CN104264227 A CN 104264227A CN 201410481465 A CN201410481465 A CN 201410481465A CN 104264227 A CN104264227 A CN 104264227A
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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
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
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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
- 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
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- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a preparation method of a gypsum crystal whisker. The preparation method comprises the following steps: by adopting waste gypsum molds of a ceramic factory as raw materials, crushing the waste gypsum molds, mixing with water to prepare gypsum slurry with a concentration of 1-30%, and then removing impurities; and adding a hydroxyapatite crystal whisker which accounts for 0.2-10% of the weight of the slurry and a gypsum crystal transformation promoter which accounts for 0.05-0.5% of the weight of the slurry into the gypsum slurry of which the impurities are removed, adding into a hydrothermal reaction kettle, and reacting for 4-12 hours under the conditions that the synthetic temperature is 100-120 DEG C, the pressure is 0.20MPa and the filling degree is 80% to obtain the gypsum crystal whisker. According to the preparation method disclosed by the invention, the gypsum crystal whisker of which the length-diameter ratio reaches 20-100 can be obtained by adopting waste gypsum of the ceramic factory as the raw material by virtue of hydrothermal synthetic transformation reaction.
Description
Technical field
The present invention relates to a kind of preparation method of crystal whisker of gypsum, be specifically related to one and discard gypsum for raw material with ceramics factory, by Hydrothermal Synthesis conversion reaction, obtain the crystal whisker of gypsum that length-to-diameter ratio reaches 20-100.
Background technology
Ceramics factory's waste gypsum mould refers in snitaryware factory, produces owing to adopting slip-casting shaping process the gypsum mold that cannot recycle in a large number formed in sanitary ware process.Because the quantity discharged of waste gypsum in Ceramic production is very large, and present the trend of cumulative year after year.Meanwhile, in a large number discarded gypsum mold is in heaps is placed in outdoor field for these, has both taken a large amount of soils, polluted underground water and leave huge potential safety hazard, and the stacking expense needing corporate payments high, is unfavorable for the sustainable development of enterprise.Therefore, the regeneration of ceramics factory's waste gypsum mould is by current extensively in addition research and apply.
Crystal whisker of gypsum refers to the fibrous single crystal of two water, half water or anhydrous calciumsulphate, has fixing shape of cross section, complete profile and perfect internal structure, is a kind of excellent property, cheap new function material.Crystal whisker of gypsum has high tensile strength and Young's modulus, can be used as the Industrial materials application of high value, and price is low, can be used in resin, rubber, coating, papermaking, making toughener or functional type filler, may be used for again abrasives, material of construction, sealing material, insulation and fire retardant material etc., have very vast potential for future development.
At present, the method preparing crystal whisker of gypsum comparative maturity both at home and abroad is mainly divided into hydrothermal method and normal pressure acidization two kinds: hydrothermal method is that dihydrate gypsum suspension massfraction being less than 2% is added in hydraulic pressure hot vessel and processes, depress at saturation steam, dihydrate gypsum becomes the semi-hydrated gypsum of tiny needle-like, again through stable crystal formation process, obtain hemihydrate calcium sulfate crystal whisker.Normal pressure acidization refers at a certain temperature, and high density dihydrate gypsum suspension can be transformed into needle-like or fibrous hemihydrate calcium sulfate crystal whisker in an acidic solution.Compared with hydrothermal method, although the method does not need reactor, and the massfraction of raw material improves greatly, and the crystal whisker of gypsum quality of synthesis is unstable, does not therefore obtain extensive application.
Summary of the invention
For the deficiencies in the prior art, the invention provides one can suitability for industrialized production, and the crystal whisker of gypsum steady quality of synthesis, realizes the preparation method of the crystal whisker of gypsum of the regeneration of ceramics factory's waste gypsum mould.
The object of the present invention is achieved like this: a kind of preparation method of crystal whisker of gypsum, comprises the following steps:
1) discard gypsum mold as raw material using ceramics factory, after mixing with water after being pulverized, be prepared into the gypsum slurry that concentration is 1-30%, remove impurity;
2) the heavy hydroxyapatite crystal whisker of 0.2-10% of slurry and the gypsum crystal inversion accelerating agent of 0.05-0.5% is added to the gypsum slurry after removal impurity, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, obtains crystal whisker of gypsum.
Described gypsum crystal inversion accelerating agent is phosphoric acid.
It is more than 90 that described ceramics factory discards gypsum mold whiteness.
The length-to-diameter ratio of described hydroxyapatite crystal whisker is 20-100.
Step 2) in the add-on of hydroxyapatite crystal whisker be the 1.2-8% that gypsum slurry adds slurry weight.
Preferably, step 2) in the add-on of hydroxyapatite crystal whisker be the 3-6% that gypsum slurry adds slurry weight.
Further preferably, step 2) in the add-on of hydroxyapatite crystal whisker be that gypsum slurry adds 5% of slurry weight.
The add-on of preferred gypsum crystal inversion accelerating agent of the present invention is gypsum slurry weight 0.1-0.4%.
Further preferably, the add-on of gypsum crystal inversion accelerating agent is gypsum slurry weight 0.2-0.3%.
The add-on of gypsum crystal inversion accelerating agent is gypsum slurry weight 0.25%.
The preparation method of crystal whisker of gypsum provided by the invention, gypsum mold is discarded as raw material using ceramics factory, in Hydrothermal Synthesis conversion reaction, by introducing hydroxyapatite crystal whisker and phosphoric acid as whisker growth promotor, prepare the crystal whisker of gypsum that length-to-diameter ratio reaches 20-100, achieve the regeneration of waste, save resource, and stably can obtain crystal whisker of gypsum.
Embodiment
Example 1: the whiteness of discarding using ceramics factory be the gypsum mold of more than 90 as raw material, be prepared into the gypsum slurry that concentration is 5% after mixing with water after being pulverized, removal impurity; To remove the gypsum slurry after impurity add length-to-diameter ratio that slurry weighs 0.2 be 50 hydroxyapatite crystal whiskers and 0.05% concentration be that the phosphoric acid of 5-15% is as gypsum crystal inversion accelerating agent, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, is undertaken reaction product filtering, dry, and the length-to-diameter ratio of the crystal whisker of gypsum obtained reaches 30-80.
Example 2: the whiteness of discarding using ceramics factory be the gypsum mold of more than 90 as raw material, be prepared into the gypsum slurry that concentration is 6% after mixing with water after being pulverized, removal impurity; Be that the phosphoric acid of 5-15% is as gypsum crystal inversion accelerating agent to removing the gypsum slurry after impurity to add length-to-diameter ratio that slurry weighs 1.2 being the hydroxyapatite crystal whisker of 70 and the concentration of 0.1%, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, is undertaken above-mentioned reaction product filtering, dry, and the length-to-diameter ratio of the crystal whisker of gypsum obtained reaches 20-90.
Example 3: the whiteness of discarding using ceramics factory be the gypsum mold of more than 90 as raw material, be prepared into the gypsum slurry that concentration is 10% after mixing with water after being pulverized, removal impurity; Be that the phosphoric acid of 5-15% is as gypsum crystal inversion accelerating agent to removing the gypsum slurry after impurity to add length-to-diameter ratio that slurry weighs 3% being the hydroxyapatite crystal whisker of 80 and the concentration of 0.3%, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, is undertaken above-mentioned reaction product filtering, dry, and the length-to-diameter ratio of the crystal whisker of gypsum obtained reaches 30-80.
Example 4: the whiteness of discarding using ceramics factory be the gypsum mold of more than 90 as raw material, be prepared into the gypsum slurry that concentration is 20% after mixing with water after being pulverized, removal impurity; Be that the phosphoric acid of 5-15% is as gypsum crystal inversion accelerating agent to removing the gypsum slurry after impurity to add length-to-diameter ratio that slurry weighs 5% being the hydroxyapatite crystal whisker of 80 and the concentration of 0.25%, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, is undertaken above-mentioned reaction product filtering, dry, and the length-to-diameter ratio of the crystal whisker of gypsum obtained reaches 20-100.
Example 5: the whiteness of discarding using ceramics factory be the gypsum mold of more than 90 as raw material, be prepared into the gypsum slurry that concentration is 30% after mixing with water after being pulverized, removal impurity; Be that the phosphoric acid of 5-15% is as gypsum crystal inversion accelerating agent to removing the gypsum slurry after impurity to add length-to-diameter ratio that slurry weighs 8% being the hydroxyapatite crystal whisker of 90 and the concentration of 0.4%, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, is undertaken above-mentioned reaction product filtering, dry, and the length-to-diameter ratio of the crystal whisker of gypsum obtained reaches 30-100.
Example 6: the whiteness of discarding using ceramics factory be the gypsum mold of more than 90 as raw material, be prepared into the gypsum slurry that concentration is 25% after mixing with water after being pulverized, removal impurity; Be that the phosphoric acid of 5-15% is as gypsum crystal inversion accelerating agent to removing the gypsum slurry after impurity to add length-to-diameter ratio that slurry weighs 10% being the hydroxyapatite crystal whisker of 100 and the concentration of 0.3%, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, is undertaken above-mentioned reaction product filtering, dry, and the length-to-diameter ratio of the crystal whisker of gypsum obtained reaches 30-90.
Claims (10)
1. a preparation method for crystal whisker of gypsum, is characterized in that: comprise the following steps:
1) discard gypsum mold as raw material using ceramics factory, after mixing with water after being pulverized, be prepared into the gypsum slurry that concentration is 1-30%, remove impurity;
2) the heavy hydroxyapatite crystal whisker of 0.2-10% of slurry and the gypsum crystal inversion accelerating agent of 0.05-0.5% is added to the gypsum slurry after removal impurity, join in hydrothermal reaction kettle, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, reaction 4-12 hour, obtains crystal whisker of gypsum.
2. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: described gypsum crystal inversion accelerating agent is phosphoric acid.
3. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: it is more than 90 that described ceramics factory discards gypsum mold whiteness.
4. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: the length-to-diameter ratio of described hydroxyapatite crystal whisker is 20-100.
5. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: step 2) in the add-on of hydroxyapatite crystal whisker be the 1.2-8% that gypsum slurry adds slurry weight.
6. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: step 2) in the add-on of hydroxyapatite crystal whisker be the 3-6% that gypsum slurry adds slurry weight.
7. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: step 2) in the add-on of hydroxyapatite crystal whisker be that gypsum slurry adds 5% of slurry weight.
8. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: the add-on of gypsum crystal inversion accelerating agent is gypsum slurry weight 0.1-0.4%.
9. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: the add-on of gypsum crystal inversion accelerating agent is gypsum slurry weight 0.2-0.3%.
10. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: the add-on of gypsum crystal inversion accelerating agent is gypsum slurry weight 0.25%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410481465.3A CN104264227A (en) | 2014-09-21 | 2014-09-21 | Preparation method of gypsum crystal whisker |
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| CN201410481465.3A CN104264227A (en) | 2014-09-21 | 2014-09-21 | Preparation method of gypsum crystal whisker |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048691A (en) * | 2018-02-05 | 2018-05-18 | 南通鑫祥锌业有限公司 | A kind of alloying metal zine plate material and preparation method thereof |
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2014
- 2014-09-21 CN CN201410481465.3A patent/CN104264227A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108048691A (en) * | 2018-02-05 | 2018-05-18 | 南通鑫祥锌业有限公司 | A kind of alloying metal zine plate material and preparation method thereof |
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Application publication date: 20150107 |