CN104278327A - Method for preparing gypsum whisker - Google Patents

Method for preparing gypsum whisker Download PDF

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Publication number
CN104278327A
CN104278327A CN201410481466.8A CN201410481466A CN104278327A CN 104278327 A CN104278327 A CN 104278327A CN 201410481466 A CN201410481466 A CN 201410481466A CN 104278327 A CN104278327 A CN 104278327A
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CN
China
Prior art keywords
gypsum
whisker
slurry
crystal whisker
crystal
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410481466.8A
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Chinese (zh)
Inventor
冯晋阳
朱万福
焦新建
祝必华
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YIDU HUIYI CERAMICS CO Ltd
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YIDU HUIYI CERAMICS CO Ltd
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Priority to CN201410481466.8A priority Critical patent/CN104278327A/en
Publication of CN104278327A publication Critical patent/CN104278327A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/62Whiskers or needles
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B7/00Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/14Single-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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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention relates to a method for preparing a gypsum whisker. The method comprises the following steps: (1) pulverizing waste gypsum molds in a ceramic factory as raw materials, mixing with water and preparing into gypsum slurry of which the concentration is 1-30% and removing impurities; and (2) adding a gypsum crystal conversion promoter which accounts for 0.2-10% of the weight of the gypsum slurry into the impurity-removal gypsum slurry to obtain a reaction product, adding the reaction product into a hydrothermal reactor, controlling the initial pH value to be 4 and reacting for 4-12 hours under the conditions that synthesis temperature is 100-120 DEG C and the degree of filling is 80% to obtain the gypsum whisker. According to the method for preparing the gypsum whisker disclosed by the invention, the waste gypsum molds in a ceramic factory are adopted as the raw materials to prepare the gypsum whisker of which the length-diameter ratio reaches 20-100 by virtue of introducing a hydroxyapatite whisker as the whisker growth promoter in a hydrothermal synthesis conversion reaction, the recycling of wastes is achieved, resources are saved and the gypsum whisker can be stably obtained.

Description

A kind of preparation method of crystal whisker of gypsum
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, just 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
The object of this invention is to provide a kind of preparation method of crystal whisker of gypsum, the method discards gypsum mold as raw material using ceramics factory, can carry out regeneration to 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 gypsum crystal inversion accelerating agent of the heavy 0.2-10% of slurry is added to the gypsum slurry after removal impurity, reactant joins in hydrothermal reaction kettle, initial ph value is 4, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, and reaction 4-12 hour, obtains crystal whisker of gypsum.
Described gypsum crystal inversion accelerating agent is hydroxyapatite crystal whisker.
The length-to-diameter ratio of described hydroxyapatite crystal whisker is 20-100.
It is more than 90 that described ceramics factory discards gypsum mold whiteness.
Step 2) in the add-on of gypsum crystal inversion accelerating agent be the 1.2-8% that gypsum slurry adds slurry weight.
Preferably, step 2) in the add-on of gypsum crystal inversion accelerating agent be the 3-6% that gypsum slurry adds slurry weight.
Further preferred, step 2) in the add-on of gypsum crystal inversion accelerating agent be that gypsum slurry adds 5% of slurry weight.
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 introduce hydroxyapatite crystal whisker be 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: discard gypsum mold as raw material using ceramics factory, is prepared into gypsum slurry that concentration be 8% after mixing after being pulverized with water, removes impurity; Gypsum slurry after removing impurity adds the gypsum crystal inversion accelerating agent that slurry weighs 0.2%, reactant joins in hydrothermal reaction kettle, initial ph value is regulated to be 4 by dripping hydrochloric acid, be 100-120 DEG C at synthesis temperature, compactedness is 80%, under the condition of pressure 0.20MPa, reaction 4-6 hour, obtaining length-to-diameter ratio is 20-80 crystal whisker of gypsum.
Example 2: discard gypsum mold as raw material using ceramics factory, is prepared into gypsum slurry that concentration be 12% after mixing after being pulverized with water, removes impurity; Gypsum slurry after removing impurity adds the gypsum crystal inversion accelerating agent that slurry weighs 2%, reactant joins in hydrothermal reaction kettle, initial ph value is regulated to be 4 by dripping hydrochloric acid, be 100-120 DEG C at synthesis temperature, compactedness is 80%, under the condition of pressure 0.20MPa, reaction 8-10 hour, obtaining length-to-diameter ratio is 30-80 crystal whisker of gypsum.
Example 3: discard gypsum mold as raw material using ceramics factory, is prepared into gypsum slurry that concentration be 20% after mixing after being pulverized with water, removes impurity; Gypsum slurry after removing impurity adds the gypsum crystal inversion accelerating agent that slurry weighs 5%, reactant joins in hydrothermal reaction kettle, initial ph value is regulated to be 4 by dripping hydrochloric acid, be 100-120 DEG C at synthesis temperature, compactedness is 80%, under the condition of pressure 0.20MPa, reaction 9-12 hour, obtaining length-to-diameter ratio is 50-100 crystal whisker of gypsum.
Example 4: discard gypsum mold as raw material using ceramics factory, is prepared into gypsum slurry that concentration be 30% after mixing after being pulverized with water, removes impurity; Gypsum slurry after removing impurity adds the gypsum crystal inversion accelerating agent that slurry weighs 10%, reactant joins in hydrothermal reaction kettle, initial ph value is regulated to be 4 by dripping hydrochloric acid, be 100-120 DEG C at synthesis temperature, compactedness is 80%, under the condition of pressure 0.20MPa, reaction 9-12 hour, obtaining length-to-diameter ratio is 50-80 crystal whisker of gypsum.
In above-described embodiment 1-4, gypsum crystal inversion accelerating agent is length-to-diameter ratio is 20-100 hydroxyapatite crystal whisker.

Claims (7)

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 gypsum crystal inversion accelerating agent of the heavy 0.2-10% of slurry is added to the gypsum slurry after removal impurity, reactant joins in hydrothermal reaction kettle, controlling initial ph value is 4, be 100-120 DEG C at synthesis temperature, pressure 0.20MPa, compactedness is under the condition of 80%, and 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 hydroxyapatite crystal whisker.
3. the preparation method of crystal whisker of gypsum according to claim 2, is characterized in that: the length-to-diameter ratio of described hydroxyapatite crystal whisker is 20-100.
4. 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.
5. the preparation method of crystal whisker of gypsum according to claim 1, is characterized in that: step 2) in the add-on of gypsum crystal inversion accelerating agent 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 gypsum crystal inversion accelerating agent 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 gypsum crystal inversion accelerating agent be that gypsum slurry adds 5% of slurry weight.
CN201410481466.8A 2014-09-21 2014-09-21 Method for preparing gypsum whisker Pending CN104278327A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105088347A (en) * 2015-08-04 2015-11-25 合肥学院 Method for utilizing solid waste ardealite to prepare gypsum whiskers

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105088347A (en) * 2015-08-04 2015-11-25 合肥学院 Method for utilizing solid waste ardealite to prepare gypsum whiskers
CN105088347B (en) * 2015-08-04 2017-06-27 合肥学院 A kind of method that utilization solid waste phosphogypsum prepares crystal whisker of gypsum

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Application publication date: 20150114

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