CN109280979A - A method of preparing semi-hydrated gypsum whisker - Google Patents

A method of preparing semi-hydrated gypsum whisker Download PDF

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Publication number
CN109280979A
CN109280979A CN201710589290.1A CN201710589290A CN109280979A CN 109280979 A CN109280979 A CN 109280979A CN 201710589290 A CN201710589290 A CN 201710589290A CN 109280979 A CN109280979 A CN 109280979A
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desulfurized gypsum
gypsum
semi
whisker
grinding
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CN201710589290.1A
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CN109280979B (en
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张晓菲
陈红霞
王霞
李帆
冉秀云
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Beijing New Building Material Group Co Ltd
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Beijing New Building Material Group Co Ltd
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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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

A method of preparing semi-hydrated gypsum whisker, which comprises selection desulfurized gypsum is raw material；The desulfurized gypsum of selection is dried, free water therein is removed；Desulfurized gypsum after drying is subjected to grinding, wears into fine-powdered；Desulfurized gypsum after grinding is sieved, large granular impurity therein is removed；Desulfurized gypsum after screening is added in certain density hydrochloric acid, slurry is stirred into, the slurry is reacted at a certain temperature；Constant pressure hydro-thermal after completion of the reaction, filters slurry；The filter cake obtained after suction filtration is washed with organic solvent；Filter cake after washing is dried to get semi-hydrated gypsum whisker is arrived.The draw ratio for the semi-hydrated gypsum whisker that the present processes are prepared has uniform diameter, and exist without lattice defects such as dislocation, stackings up to 300.

Description

A method of preparing semi-hydrated gypsum whisker
Technical field
This application involves but be not limited to inolrganic chemicals preparation field, be more particularly without limitation, to a kind of prepare half water stone The method of cream whisker.
Background technique
Semi-hydrated gypsum whisker is the fibrous monocrystal of half-H 2 O calcium sulphate, has high tensile strength, elasticity modulus, height Dielectric strength, while abrasion performance, high temperature resistant, corrosion-resistant, infrared reflectivity are good, are easy to be surface-treated and high molecular polymerization The affinity of object is strong, is a kind of inorganic material cheap, comprehensive performance is high, can be used as enhancing component and is applied to tree Rouge, rubber in coating, there is extremely vast potential for future development.
The traditional preparation methods of semi-hydrated gypsum whisker are mainly steam pressure hydro-thermal method, have mainly been added to dihydrate gypsum and have turned It in the salting liquid of brilliant agent, is reacted under high pressure-temperature, this method the high requirements on the equipment, complicated for operation, energy consumption is high.
Summary of the invention
It is the general introduction to the theme being described in detail herein below.This general introduction is not the protection model in order to limit claim It encloses.
This application provides it is a kind of normal pressure, without crystal modifier under conditions of using desulfurized gypsum prepare semi-hydrated gypsum whisker Method.
Specifically, this application provides a kind of methods for preparing semi-hydrated gypsum whisker.
The provided herein method for preparing semi-hydrated gypsum whisker the following steps are included:
Feeding: selection desulfurized gypsum is raw material；
It is dry: the desulfurized gypsum of selection being dried, free water therein is removed；
Grinding: the desulfurized gypsum after drying is subjected to grinding, wears into fine-powdered；
Screening: the desulfurized gypsum after grinding is sieved, large granular impurity therein is removed；
Constant pressure hydro-thermal reaction: the desulfurized gypsum after screening being added in certain density hydrochloric acid, slurry is stirred into, The slurry is reacted at a certain temperature；
Filter: constant pressure hydro-thermal after completion of the reaction, filters slurry；
Washing: the filter cake obtained after suction filtration is washed with organic solvent；
It is dry: the filter cake after washing to be dried to get semi-hydrated gypsum whisker is arrived.
In presently filed embodiment, the described desulfurized gypsum of selection is dried can be the desulfurization stone that will be chosen Cream dry 4-6h at 40-50 DEG C.
In presently filed embodiment, the screening can be that 100-300 mesh is sieved.
In presently filed embodiment, the concentration of the hydrochloric acid can be 2mol/L.
In presently filed embodiment, the mass ratio of desulfurized gypsum and hydrochloric acid after the screening can be 1:(8- 11)。
In presently filed embodiment, the reaction temperature of the constant pressure hydro-thermal reaction can be 93-96 DEG C, the reaction time It can be 6-8h.
In presently filed embodiment, the organic solvent can be dehydrated alcohol.
In presently filed embodiment, the drying temperature of the filter cake can be 93-96 DEG C, and drying time can be 4- 6h。
By the present processes can normal pressure, without crystal modifier under conditions of realize semi-hydrated gypsum whisker preparation, and And the draw ratio of the semi-hydrated gypsum whisker of preparation has uniform diameter up to 300, HRTEM image shows that it does not have dislocation, stacking Equal lattice defects exist, and the control to product crystal phase, pattern are realized, to the preparation method and industry of the following semi-hydrated gypsum whisker Solid waste desulfurized gypsum recycles offer guidance.
Other features and advantage will illustrate in the following description, also, partly become from specification It obtains it is clear that being understood and implementing the application.The purpose of the application and other advantages can be by specifications, right Specifically noted structure is achieved and obtained in claim and attached drawing.
Detailed description of the invention
Attached drawing is used to provide to further understand technical scheme, and constitutes part of specification, with this The embodiment of application is used to explain the technical solution of the application together, does not constitute the limitation to technical scheme.
Fig. 1 is the XRD diagram of desulfurized gypsum raw material.
Fig. 2 a)-b) it is SEM figure of the desulfurized gypsum raw material under different amplification.
Fig. 3 is the XRD diagram of semi-hydrated gypsum whisker prepared by the embodiment of the present application 1.
Fig. 4 is the SEM figure of semi-hydrated gypsum whisker prepared by the embodiment of the present application 1.
Fig. 5 is the TEM figure of semi-hydrated gypsum whisker prepared by the embodiment of the present application 1.
Fig. 6 is the HRTEM figure of semi-hydrated gypsum whisker prepared by the embodiment of the present application 1.
Specific embodiment
For the purposes, technical schemes and advantages of the application are more clearly understood, below in conjunction with attached drawing to the application Embodiment be described in detail.It should be noted that in the absence of conflict, in the embodiment and embodiment in the application Feature can mutual any combination.
Desulfurized gypsum used in following embodiment derives from Zhongweiof Ningxia, northwest China power plant, other raw materials and reagents, such as nothing It illustrates, is ordinary commercial products.
Embodiment 1:
A. the selection of raw material: selection 2g desulfurized gypsum is raw material.
B. the drying of raw material: sending the desulfurized gypsum of selection into drying box, and the temperature for adjusting drying box is 40 DEG C, dry 4h removes the free water in raw material.
C. the grinding of raw material: the desulfurized gypsum after drying is subjected to grinding in mortar, wears into fine-powdered.
D. the screening of raw material: the desulfurized gypsum after grinding is crossed into 230 meshes and is sieved, it is miscellaneous to remove bulky grain therein Matter.
E. the constant pressure hydro-thermal reaction of raw material: the desulfurized gypsum obtained after 1g screening is weighed, the 2mol/ of 10ml is added it to In the hydrochloric acid of L (density is about 1.03g/ml), 6h is reacted at 93 DEG C.
F. it filters: the slurry after reaction being subjected to rapid filtration under suction, obtains white filter cake.
G. it washs: the filter cake obtained after suction filtration being washed with dehydrated alcohol at room temperature.
H. it dries: the filter cake after washing is sent into drying box, the temperature for adjusting drying box is 93 DEG C, dries 4h to get arriving Semi-hydrated gypsum whisker.
Embodiment 2:
A. the selection of raw material: selection 4g desulfurized gypsum is raw material.
B. the drying of raw material: sending the desulfurized gypsum of selection into drying box, and the temperature for adjusting drying box is 45 DEG C, dry 5h removes the free water in raw material.
C. the grinding of raw material: the desulfurized gypsum after drying is subjected to grinding in mortar, wears into fine-powdered.
D. the screening of raw material: the desulfurized gypsum after grinding is crossed into 240 meshes and is sieved, it is miscellaneous to remove bulky grain therein Matter.
E. the constant pressure hydro-thermal reaction of raw material: the desulfurized gypsum obtained after 3g screening is weighed, the 2mol/ of 26ml is added it to In the hydrochloric acid of L, 7h is reacted at 95 DEG C.
F. it filters: the slurry after reaction being subjected to rapid filtration under suction, obtains white filter cake.
G. it washs: the filter cake obtained after suction filtration being washed with dehydrated alcohol at room temperature.
H. it dries: the filter cake after washing is sent into drying box, the temperature for adjusting drying box is 95 DEG C, dries 5h to get arriving Semi-hydrated gypsum whisker.
Embodiment 3:
A. the selection of raw material: selection 10g desulfurized gypsum is raw material.
B. the drying of raw material: sending the desulfurized gypsum of selection into drying box, and the temperature for adjusting drying box is 50 DEG C, dry 6h removes the free water in raw material.
C. the grinding of raw material: the desulfurized gypsum after drying is subjected to grinding in mortar, wears into fine-powdered.
D. the screening of raw material: the desulfurized gypsum after grinding is crossed into 240 meshes and is sieved, it is miscellaneous to remove bulky grain therein Matter.
E. the constant pressure hydro-thermal reaction of raw material: the desulfurized gypsum obtained after 8g screening is weighed, the 2mol/ of 80ml is added it to In the hydrochloric acid of L, 8h is reacted at 96 DEG C.
F. it filters: the slurry after reaction being subjected to rapid filtration under suction, obtains white filter cake.
G. it washs: the filter cake obtained after suction filtration being washed with dehydrated alcohol at room temperature.
H. it dries: the filter cake after washing is sent into drying box, the temperature for adjusting drying box is 96 DEG C, dries 6h to get arriving Semi-hydrated gypsum whisker.
Test case
1, desulfurized gypsum raw material and the application are tested using SHIMADZU XRD-7000 type X-ray diffraction analysis instrument respectively The XRD spectrum of semi-hydrated gypsum whisker prepared by embodiment 1.
Test condition: Cu target K alpha ray source, tube voltage 40kV, tube current 30mA, sweep speed are 2 °/min.Test As a result see Fig. 1 and Fig. 3.
The variation of comparison diagram 1 and Fig. 3, XRD characteristic peak position illustrate desulfurized gypsum through method described in the embodiment of the present application 1 After conversion, object mutually becomes half-H 2 O calcium sulphate from calcium sulphate dihydrate.
2, it tests desulfurized gypsum raw material respectively using S-4800 field emission scanning electron microscope (FESEM) and the application is real Apply SEM figure of the semi-hydrated gypsum whisker of the preparation of example 1 under different amplification.
Test condition: acceleration voltage 15kV.Test result is see Fig. 2 and Fig. 4.
After comparison diagram 2 and Fig. 4 can be seen that desulfurized gypsum method conversion described in the embodiment of the present application 1, microscopic appearance Threadiness is changed by large grained.
3, the semi-hydrated gypsum whisker of the preparation of the embodiment of the present application 1 is tested using JEM-2010 type transmission electron microscope TEM figure.Test result is see Fig. 5.
From fig. 5, it can be seen that semi-hydrated gypsum whisker prepared by the embodiment of the present application 1 has uniform diameter.
The average length for the semi-hydrated gypsum whisker prepared is about 500-600 μm, and average diameter is about 1-2 μm, draw ratio About 300.
4, the semi-hydrated gypsum whisker of the preparation of the embodiment of the present application 1 is tested using JEM-2010 type transmission electron microscope HRTEM figure.Test result is see Fig. 6.
From fig. 6, it can be seen that semi-hydrated gypsum whisker prepared by we's application embodiment 1 has clearly lattice fringe, do not have With the presence of the lattice defects such as dislocation, stacking, spacing of lattice 0.341nm, (020) crystal face corresponding to half-H 2 O calcium sulphate.
Although embodiment disclosed by the application is as above, the content only for ease of understanding the application and use Embodiment is not limited to the application.Technical staff in any the application fields, is taken off not departing from the application Under the premise of the spirit and scope of dew, any modification and variation, but the application can be carried out in the form and details of implementation Scope of patent protection, still should be subject to the scope of the claims as defined in the appended claims.

Claims (8)

1. a kind of method for preparing semi-hydrated gypsum whisker, the described method comprises the following steps:
Feeding: selection desulfurized gypsum is raw material；
It is dry: the desulfurized gypsum of selection being dried, free water therein is removed；
Grinding: the desulfurized gypsum after drying is subjected to grinding, wears into fine-powdered；
Screening: the desulfurized gypsum after grinding is sieved, large granular impurity therein is removed；
Constant pressure hydro-thermal reaction: the desulfurized gypsum after screening is added in certain density hydrochloric acid, slurry is stirred into, by institute Slurry is stated to be reacted at a certain temperature；
Filter: constant pressure hydro-thermal after completion of the reaction, filters slurry；
Washing: the filter cake obtained after suction filtration is washed with organic solvent；
It is dry: the filter cake after washing to be dried to get semi-hydrated gypsum whisker is arrived.
2. according to the method described in claim 1, wherein, the desulfurization desulfurized gypsum of selection being dried will to choose Gypsum dry 4-6h at 40-50 DEG C.
3. according to the method described in claim 1, wherein, the screening was that 100-300 mesh is sieved.
4. according to the method described in claim 1, wherein, the concentration of the hydrochloric acid is 2mol/L.
5. method according to claim 1 or 4, wherein the mass ratio of desulfurized gypsum and hydrochloric acid after the screening is 1: (8-11)。
6. the reaction temperature of the constant pressure hydro-thermal reaction is 93-96 DEG C according to the method described in claim 1, wherein, when reaction Between be 6-8h.
7. according to the method described in claim 1, wherein, the organic solvent is dehydrated alcohol.
8. according to the method described in claim 1, wherein, the drying temperature of the filter cake is 93-96 DEG C, drying time 4- 6h。
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111607827A (en) * 2019-07-16 2020-09-01 北新集团建材股份有限公司 Post-treatment method of calcium sulfate whisker
CN112760716A (en) * 2021-01-15 2021-05-07 海南蓝岛环保产业股份有限公司 Phosphorus-containing desulfurized gypsum recycling treatment method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111607827A (en) * 2019-07-16 2020-09-01 北新集团建材股份有限公司 Post-treatment method of calcium sulfate whisker
CN111607827B (en) * 2019-07-16 2022-01-07 北新集团建材股份有限公司 Post-treatment method of calcium sulfate whisker
CN112760716A (en) * 2021-01-15 2021-05-07 海南蓝岛环保产业股份有限公司 Phosphorus-containing desulfurized gypsum recycling treatment method
CN112760716B (en) * 2021-01-15 2024-05-24 海南蓝岛环保产业股份有限公司 Recycling treatment method of phosphogypsum

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