CN100523312C - Preparation method of calcium sulfate whisker - Google Patents
Preparation method of calcium sulfate whisker Download PDFInfo
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- CN100523312C CN100523312C CNB2005100474526A CN200510047452A CN100523312C CN 100523312 C CN100523312 C CN 100523312C CN B2005100474526 A CNB2005100474526 A CN B2005100474526A CN 200510047452 A CN200510047452 A CN 200510047452A CN 100523312 C CN100523312 C CN 100523312C
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- calcium sulfate
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- dolicho
- crystallizing
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Abstract
This invention relates to a preparation of crystal whisker of calcium sulfate, particularly relating a preparation that produces fibriform mon-crystal of half water or dried gypsum, its concrete steps as following: (1) Adopt hydrothermal synthesis etc technology to compose target agent of crystallizing; (2) Firstly calcium oxide that is technica grade is pretreated, added into reaction vessel to digest at 40-60DEG C, calcarea galacta is obtained; (3) The calcarea galacta that is obtained raises temperature to 40-110DEG C in reaction vessel, add equimolar solution of sulphuric acid, mix 30-60min,add targeting agent of crystallizing in reaction process. Make it react sufficiently, obtain products of required crystal whisker of calcium sulfate by filtering, cleaning, surface treatment and drying. Characteristic of this invention is: add targeting agent of crystallizing that is self produced, control different reactive temperature, obtain crystal whisker of calcium sulfate with different dolicho- diameter ratio, dolicho- diameter of this product is uniform, dolicho- diameter ratio is large, purity of raw material has no strict requirement.
Description
Technical field
The present invention relates to a kind of Preparation methods of gypsum whiskers method, particularly a kind of production half water, the fibrous mcl method of anhydrous calciumsulphate.
Background technology
Whisker is meant to have the fixed cross-sectional area, complete profile, and perfect internal structure, length-to-diameter ratio is up to 5～1000 fibrous single crystal.Because its diameter is little, atomic arrangement high-sequential when crystallization has changed the space that conventional material has and the defective of dislocation.Therefore, calcium sulfate crystal whiskers has unique premium properties.The weighting agent that can be used as medium tenacity, the reinforcing effect of the reinforcing effect of small diameter fiber and other high-performance fiber strongthener is approaching.With its enhanced plastics, tensile strength, flexural strength, crooked elastic rate and heat-drawn wire are improved.It can replace asbestos to make friction materials, material of construction, insulation, cold insulation material etc.Also can partly replace glass fibre.Moisture whisker can only be lower than 176.7 ℃ of uses down, and the use temperature of anhydrous whisker is up to 1000 ℃.
Calcium sulfate crystal whiskers normally is raw material with the gypsum, and building-up process is the process that the plaster stone of other shapes is transformed into fibrous calcium sulphate hemihydrate.Reaction process is as follows:
CaSO
42H
2O → CaSO
41/2H
2O+3/2 H
2O (reaction conditions heating)
The calcium sulfate crystal whiskers of half water is dried to 200 ℃ and obtains anhydrous calcium sulfate crystal whiskers.
Water thermal crystallization synthetic calcium sulfate crystal whiskers, its shortcoming be need be very high temperature, pressure, and productive rate can not reach 100%.
Summary of the invention
The object of the present invention is to provide a kind of material purity and temperature condition requirement low, Synthesis conversion height, the calcium sulphate crystal whisker preparation method that length-to-diameter ratio is high.
Technical solution of the present invention can realize according to following mode:
The Preparation methods of gypsum whiskers method, can carry out successively as follows:
(1) synthetic crystallization director; Described crystallization director is for adopting the calcium sulfate crystal whiskers of hydrothermal synthesis method preparation;
(2) the pre-treatment of technical grade calcium oxide elder generation, put into reactor 40～60 ℃ of digestion, obtain lime slurry;
(3) the gained lime slurry is warming up to 40～110 ℃ in reactor, adds and the equimolar sulphuric acid soln of calcium oxide, stirred 30～60 minutes, in the process of reaction, add crystallization director, it is fully reacted; The add-on of described crystallization director is counted 1% of theoretical product growing amount with weight percentage;
(4) after filtration washing,, surface treatment and drying obtain required calcium sulfate crystal whiskers product.
Above-mentioned crystallization director is to adopt hydro-thermal synthetic.Massfraction is added in the water heater less than 2% dihydrate gypsum suspension handles, depress at saturation steam, dihydrate gypsum becomes tiny acicular semi-hydrated gypsum, again through the stable crystal form processing, obtains the calcium sulfate crystal whiskers of prepared such as sulfate hemihydrate calcium pyroborate.
The acid-base neutralisation reaction takes place by the calcium oxide digestion process of technical grade in the present invention, adds crystallization director, obtains the calcium sulfate crystal whiskers product through filtration, washing, surface treatment, drying process.Characteristics of the present invention are: add homemade crystallization director, the different temperature of reaction of control, obtain the calcium sulfate crystal whiskers of different length-to-diameter ratios, this product major diameter homogeneous, length-to-diameter ratio be big, material purity is not strict with.And resultant whisker productive rate 100%.The waste water that produces is easy to handle, and helps environment protection.
Description of drawings
Below in conjunction with drawings and Examples operational path of the present invention is further described.
Fig. 1 is the X-ray diffraction spectrogram of the resultant product of the present invention;
Fig. 2 is the resultant product electron microscope picture of the present invention.
Embodiment
Embodiment 1
Technical grade CaO is taken by weighing 100g put into reactor, add 500ml distilled water, pre-treatment in ultrasonic wave is fully pulverized macrobead, adds 500ml distilled water again, 40～60 ℃ of following digestion process.Obtain lime slurry, be warmed up to 80 ℃, add and the equimolar sulphuric acid soln of calcium oxide, in reaction process, add homemade crystallization director, add-on is 1% of a theoretical product growing amount, stirs 40min, and it is fully reacted, reaction soln is suction filtration separation as early as possible while hot, and the X-ray diffraction spectrogram of resultant product and electron microscope picture are as shown in Figure 1 and Figure 2.
The calcium sulfate crystal whiskers product of gained need carry out different finishinges according to the object difference of using, and it is well melted mutually with other materials.Be convenient to bring into play its performance.
Embodiment 2
Except that temperature of reaction was 40 ℃, it was identical with embodiment 1 to add homemade crystallization director 2% other conditions.
Embodiment 3
Except that temperature of reaction is 60 ℃, it is identical with embodiment 1 to add crystallization director 3% other conditions.
Embodiment 4
Except that 90 ℃ of temperature of reaction, it is identical with embodiment 1 to add crystallization director 0.5% other conditions.
Embodiment 5
Except that 100 ℃ of temperature of reaction, other conditions are identical with embodiment 1.
Embodiment 6
Except that 110 ℃ of temperature of reaction, add crystallization director 2%, other conditions are identical with embodiment 1.
| Embodiment | Yield % | Length-to-diameter ratio |
| Embodiment 1 | 100 | 190∶1 |
| Embodiment 2 | 100 | 40∶1 |
| Embodiment 3 | 100 | 120∶1 |
| Embodiment 4 | 100 | 240∶1∶ |
| Embodiment 5 | 100 | 320∶1 |
| Embodiment 6 | 100 | 400∶1 |
Waste water of the present invention is settled solution, does not contain hazardous substance, and it is acid that solution shows slightly, and adds 5% sodium hydroxide solution, adds through three grades of settling tanks.Can discharge, be easy to handle, be beneficial to environment protection.Need to prove that protection scope of the present invention is not restricted to the described embodiments.
Claims (1)
1, the Preparation methods of gypsum whiskers method is characterized in that, carries out successively as follows:
(1) synthetic crystallization director; Described crystallization director is for adopting the calcium sulfate crystal whiskers of hydrothermal synthesis method preparation;
(2) the pre-treatment of technical grade calcium oxide elder generation, put into reactor 40～60 ℃ of digestion, obtain lime slurry;
(3) the gained lime slurry is warming up to 40～110 ℃ in reactor, adds and the equimolar sulphuric acid soln of calcium oxide, stirred 30～60 minutes, in the process of reaction, add crystallization director, it is fully reacted; The add-on of described crystallization director is counted 1% of theoretical product growing amount with weight percentage;
(4) after filtration washing,, surface treatment and drying obtain required calcium sulfate crystal whiskers product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100474526A CN100523312C (en) | 2005-10-19 | 2005-10-19 | Preparation method of calcium sulfate whisker |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100474526A CN100523312C (en) | 2005-10-19 | 2005-10-19 | Preparation method of calcium sulfate whisker |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1955345A CN1955345A (en) | 2007-05-02 |
| CN100523312C true CN100523312C (en) | 2009-08-05 |
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ID=38062888
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| CNB2005100474526A Expired - Fee Related CN100523312C (en) | 2005-10-19 | 2005-10-19 | Preparation method of calcium sulfate whisker |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101311337B (en) * | 2008-04-25 | 2010-06-16 | 东北大学 | Process for preparing calcium sulphate whiskers by using flue gas desulfurization gypsum |
| CN101319382B (en) * | 2008-06-25 | 2011-04-27 | 国家***天津海水淡化与综合利用研究所 | Calcium sulphate crystal whisker preparation method with sea water bittern as raw material |
| CN101792932B (en) * | 2009-11-16 | 2012-04-18 | 瓮福（集团）有限责任公司 | Method for preparing ultra-fine calcium sulfate crystal whisker by using phosphogypsum |
| CN102286783B (en) * | 2011-09-30 | 2013-05-22 | 瓮福（集团）有限责任公司 | New method for preparing calcium sulfate whiskers |
| CN103510151B (en) * | 2013-08-30 | 2014-11-19 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulfate whiskers from dolomite |
| CN103938263B (en) * | 2014-04-09 | 2016-08-31 | 南京科硕生化科技有限公司 | The technique preparing calcium sulfate crystal whiskers with cyanogen imines S,S-Dimethyl cyanoimidodithiocarbonate waste water |
| CN109499958B (en) * | 2018-10-19 | 2021-04-13 | 中国石油化工集团有限公司 | Efficient cleaning process for calcium sulfate whisker precursor with high chloride ion content |
-
2005
- 2005-10-19 CN CNB2005100474526A patent/CN100523312C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 半水高强度石膏生产新工艺. 李天文.现代化工. 1998 |
| 半水高强度石膏生产新工艺. 李天文.现代化工. 1998 * |
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| CN1955345A (en) | 2007-05-02 |
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Granted publication date: 20090805 Termination date: 20091119 |