CN1598083A - Process for preparing calcium sulfate whisker - Google Patents
Process for preparing calcium sulfate whisker Download PDFInfo
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- CN1598083A CN1598083A CN 200410050288 CN200410050288A CN1598083A CN 1598083 A CN1598083 A CN 1598083A CN 200410050288 CN200410050288 CN 200410050288 CN 200410050288 A CN200410050288 A CN 200410050288A CN 1598083 A CN1598083 A CN 1598083A
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Abstract
This invention is a preparation method of calcium sulfate crystal whisker. The material is plaster stone (CaSO4.2H2O) and water in the entire production. After raw material preparation, building up reactions, dehydrate, refine and edulcoration. Its characteristic is that the active content of plaster stone up to above 95%, the whiteness is above 90%. Mixed with water and turn into plaster stone slime, then put them into reactor to make them have chemical reaction, then on the other procedures. The calcium sulfate crystal whisker made by this method has good performance, low cost, and can be used in all kinds of industries.
Description
Affiliated technical field
This invention belongs to mineral processing, field of non-metallic materials, is specially a kind of Preparation methods of gypsum whiskers method.
Background technology
Whisker be meant have the fixed shape of cross section, complete profile, perfect internal structure, length-to-diameter ratio be up to the fibrous single crystal of 5-1000, is enhancing constituent element the most high-grade in the matrix material.With the whisker is to strengthen the matrix material that constituent element can make excellent performance.
Industrially developed country such as the U.S., Japan very payes attention to the research and development of whisker, existing multiple whisker has obtained application, for example class whiskers such as silicon carbide, silicon nitride are joined among the pottery, can significantly improve the intensity and the toughness of stupalith, but price is very expensive, 900 dollars/kilogram of the silicon carbide whisker prices that Japanese East Sea carbide company is produced.From phase early 1980s, China's emphasis is studied whiskers such as silicon carbide, silicon nitrides, has obtained breakthrough progress.The price of homemade silicon carbide whisker is that 3000-5000 unit/kilogram is suitable substantially with international price.Because the selling at exorbitant prices of whisker, its Application Areas is greatly limited.Thereby the advantage of performance China aspect non-metallic mineral resource researched and developed cheap whisker, and be for industries such as plastics, rubber, coating, friction materials provide high-quality strongthener (additive), significant.
Calcium sulfate crystal whiskers is to be raw material with natural plaster stone, half water, anhydrous, the dead roasting ca sulphate fibre shape single crystal that adopt advanced technology and prescription to produce.Calcium sulfate crystal whiskers has uniform structure, complete profile, specific cross section, stable size, and its average aspect ratio can reach 50～80.Calcium sulfate crystal whiskers with other staple fibre relatively high physical strength is arranged, and price is minimum in the whisker industry, the unrivaled ratio of performance to price of other whisker is arranged, so range of application has very broad application prospect.
The main raw material that generates calcium sulfate crystal whiskers is a plaster stone.China has abundant plaster stone resource, cheap, is the synthetic calcium sulfate crystal whiskers of raw material with the plaster stone, the type material of excellent property both is provided for matrix material and other relevant industrial departments, also opened up new approach simultaneously for the further deep processing of plaster stone.
Research about calcium sulfate crystal whiskers, abroad just set about in the seventies in 20th century as Japan, the U.S., Germany etc., but because the calcium sulfate crystal whiskers process of growth is subjected to such environmental effects more, growth conditions is difficult to control, has increased the difficulty of calcium sulfate crystal whiskers research to a certain extent.To the eighties in 20th century, the research work of calcium sulfate crystal whiskers has obtained breakthrough, but because calcium sulfate crystal whiskers when in downstream product, using, modification of itself or adding technology need to explore and improve too, and applying of calcium sulfate crystal whiskers is obstructed.In addition, European and American areas Gypsum Mine natural resources shortage comprises other all restriction conditions and contradiction, makes external research to calcium sulfate crystal whiskers rest on the pilot scale stage always, does not have suitability for industrialized production.
China just began calcium sulfate crystal whiskers is studied from phase late 1980s, was to start late.At present, the domestic method for preparing calcium sulfate crystal whiskers mainly contains following three kinds:
(1) the hot method of hydraulic pressure.The hot method of hydraulic pressure is weight concentration to be added in the water autoclave less than 2% terra alba suspension handle, and depresses at saturation steam, and terra alba becomes tiny acicular calcium sulphate hemihydrate, again through the stable crystal form processing, obtains the sulfate hemihydrate calcium pyroborate.This method production cost height, application is restricted.
(2) normal pressure acidization.The normal pressure acidization is meant at a certain temperature, allows high density terra alba suspension in acidic solution, can be transformed into needle-like or fibrous sulfate hemihydrate calcium pyroborate.The calcium sulfate crystal whiskers length of producing in this way is 100～200 μ m, diameter 1～4 μ m.Compare with the hot method of hydraulic pressure, do not need autoclave, and the raw materials quality mark improves greatly, cost significantly reduces, and is easy to suitability for industrialized production.
(3) be the feedstock production calcium sulfate crystal whiskers with the halogen slag.The preparation raw material is: bittern, density are 1.262g/cm
3, industrial waste acid contains sulfur waste acid 1～2mol/cm
3, technical grade CaO (content＞95%).The calcium sulfate crystal whiskers length of producing in this way is 50～100 μ m, diameter 1～4 μ m.
The problem that prior art exists:
(1) the hot method material concentration of hydraulic pressure low (less than 2%), explained hereafter cost height is difficult for industrialized production.
(2) a large amount of sulfuric acid that use in the normal pressure acidization technological process are serious to equipment corrosion, also can produce a large amount of acid-bearing wastewaters simultaneously, and environment is had severe contamination.
(3) be feedstock production calcium sulfate crystal whiskers technology with the halogen slag, the raw material that is adopted has certain influence to product performance index.
(4) diameter of the calcium sulfate crystal whiskers that makes of above-mentioned all technologies is all at micron order.
Summary of the invention
According to the defective of present calcium sulfate crystal whiskers technology of preparing, the objective of the invention is to seek a kind of novel method of calcium sulfate crystal whiskers preparation, prepare the calcium sulfate crystal whiskers product of diameter in 0.001～4 μ m, length 50～200 μ m, diameter and length controlled; Enhance productivity and throughput, reduce the production cost of calcium sulfate crystal whiskers, satisfy the active demand of society this kind material with this.
The particular content of this invention is: with plaster stone (CaSO
42H
2O) and water be raw material, adopt operation control preparation technology's flow process simple, that be easy to transform to make calcium sulfate crystal whiskers.
Concrete preparation method of the present invention is divided into raw material preparation, building-up reactions substantially, dehydrates and an operation such as refining and edulcoration as shown in Figure 1, and final production goes out qualified calcium sulfate crystal whiskers.The particular content of each operation comprises:
(1) raw material is prepared.Select (CaSO
42H
2O) effective content reaches more than 95, whiteness is at plaster stone more than 90% and tap water.Be mixed with concentration by weight percentage at normal temperatures and be 4～14% plaster stone slip, handle through mulser, it is fully emulsified that slurry is obtained;
(2) building-up reactions.Slurry after the emulsification is joined in the synthesis reactor,, add pH adjustment agent and make solution reach certain potential of hydrogen, and, make it fully to carry out chemical reaction under certain temperature and pressure, constantly stirring then according to specific requirement.Wherein adopt following parameter, can obtain the ideal effect, that is: temperature of reaction: 100～200 ℃; Reaction pressure: 1～3atm; Add pH and adjust agent, make the pH value of solution value reach 8～12; Reaction times: 30～45min; Stirring velocity: 400～1000rpm.
Thereby prepare the calcium sulfate crystal whiskers intermediates;
(3) filter.Utilize box filter or centrifugal filter to filter through the calcium sulfate crystal whiskers intermediates that prepared in reaction goes out, the water content of filtering products obtained therefrom is about 40% (weight percent concentration).
(4) drying.Adopt compartment dryer to carry out the static state drying, also can adopt flash dryer to carry out dynamic drying, drying temperature is 200～400 ℃, and the calcium sulfate crystal whiskers product water content after drying is handled is less than 0.5% (weight percent).
(5) refinement treatment.In order to obtain the calcium sulfate crystal whiskers product of favorable dispersity, general employing is broken up equipment the dry products obtained therefrom of static state is broken up processing, thereby obtains the ideal calcium sulfate crystal whiskers.
(6) surface modification.Surface modification is meant with methods such as physics, chemistry, machineries material surface handled, and on purpose changes the physicochemical property of material surface according to application need, to satisfy demands of applications.The calcium sulfate crystal whiskers surface modification adopts stearic acid or titanic acid ester as surface-modifying agent, uses high-speed mixer as surface modification equipment.The consumption of surface-modifying agent is 1.0～3.0%.Whether carrying out the calcium sulfate crystal whiskers surface modification will decide because of need.Product after exquisiteness processing and surface modification can be packed and dispatch from the factory.
In actual production, if adopt different operating parameterss, as the concentration of temperature, pressure, gypsum emulsion, reaction emulsion initial pH value, stirring velocity etc., the i.e. diameter of may command calcium sulfate crystal whiskers product and length.With reaction emulsion initial pH value is that example is described as follows: when the pH value was 3～5, diameter of whiskers was 1330nm, and length-to-diameter ratio is 100～200; When the pH value was 7～9, diameter of whiskers was 730nm, and length-to-diameter ratio is 80～200; When the pH value was 9～12, diameter of whiskers can drop to below the 100nm, and length-to-diameter ratio is 50～200, changed other operating parameters and also can receive certain regulating effect.
Calcium sulfate crystal whiskers is made by hydrothermal method, it be emulsion with terra alba and water in the closed stainless steel reactor, constantly stir, be heated to certain temperature, reach certain pressure after and generate.Simultaneously, use the diameter and the length of suitable additive control calcium sulfate crystal whiskers.The essence of preparation process is the conversion process of granular gypsum to fibrous semi-hydrated gypsum, and its reaction equation is as follows:
After reaction is finished, to product filter, drying, form anhydrous calcium sulfate whisker.Reaction equation is as follows:
Invention effect (product index and technology outstanding feature)
(1) product index
Density: 2.96g/cm
3Aerated density: 0.1-0.4g/cm
3
Length: 50-200 μ m diameter: 0.001-4 μ m
Fusing point: 1450 ℃ of tensile strength: 20.5GPa
Tensile modulus: 178GPa refractive index: 1.585
Water-soluble (22 ℃):＜1200ppm Mohs intensity: 3-4
The technology of the present invention is compared with other calcium sulfate crystal whiskers preparation technology, has following outstanding feature:
1. the diameter of calcium sulfate crystal whiskers is 0.001～4 μ m., length 50～200 μ m, adopt different operating parameterss by in producing, as the concentration of temperature, pressure, gypsum emulsion, reaction initial pH value, stirring velocity etc., can control the diameter and the length of calcium sulfate crystal whiskers product, both can prepare diameter is nano level calcium sulfate crystal whiskers product, can prepare diameter again at micron-sized calcium sulfate crystal whiskers product.
2. the gypsum emulsion concentration can reach 4～14%, has improved throughput greatly.
Calcium sulfate crystal whiskers product diameter, length is even, quality is high.
4. production technique environmentally safe; Eliminated the shortcoming that the normal pressure acidization uses sulfuric acid that equipment and environment are worked the mischief in a large number.
5. technology is simple, and production cost is low, is easy to suitability for industrialized production.
The calcium sulfate crystal whiskers product performance are good, and are with low cost, obtained using widely in every profession and trade, have vast market prospect.
(1) be used for friction materials: the friction materials industry of China still is extensive use of asbestos at present, because asbestos are poisonous, its dust can cause multiple diseases such as lung cancer, bronchogenic carcinoma, and western developed country has been prohibited and use asbestos in friction materials, particularly the friction plate of car.And calcium sulfate crystal whiskers is nontoxic, is suitable as the surrogate of asbestos.
(2) as strengthening constituent element: calcium sulfate crystal whiskers can be used as the enhancing constituent element of plastics, rubber, urethane, metal and pottery.After in plastics, adding calcium sulfate crystal whiskers, can improve physical strength, thermotolerance, the dimensional stability of material.Strengthening goods can be widely used in improving its correlated performance in the part of machinery, electronics, chemical plant installations.
(3) be used for environmental engineering: the aerated density of calcium sulfate crystal whiskers is minimum, has bigger specific surface area, and calcium sulfate crystal whiskers is nontoxic, is particularly suitable for the filtration of beverage, medicine.When using calcium sulfate crystal whiskers to filter high temperature or corrosive liquid or gas, before filtering, needn't cool off or neutralize, but can directly filter.Also can be used as filtering material and remove detrimental impurity in waste gas and the waste water.
(4) be used for asphalt modification: calcium sulfate crystal whiskers can be used for pitch filler and toughener, and calcium sulfate crystal whiskers has decisive influence to improving the bituminous softening temperature.
(5) be used for coating and paint: the coating and strong, high temperature resistant, the good insulating of paint adhesive ability that add calcium sulfate crystal whiskers.
(6) weighting agent: in paper, add calcium sulfate crystal whiskers and can improve its opacity, plasticity-, flame retardant resistance and printing performance.
Description of drawings
Fig. 1 prepares the principle process flow sheet for calcium sulfate crystal whiskers.
Embodiment
(1) example 1
Raw material is selected from Hubei Province, and the main secondary element of raw material is Ca, S, and impurity is Mg, Si, Al, Fe etc., plaster stone (CaSO in the raw material
42H
2O) content is 98%.It is 4～14% slip that gypsum powder and water are mixed with weight concentration, after mulser emulsification, adds autoclave, after the sealing, starts stirring, and stirring velocity is 400～1000rpm, and begins heating.The solution temperature of calcium sulfate crystal whiskers building-up process in the temperature sensor measurement reactor, the pressure in the adopts pressure sensor assaying reaction still.When temperature of reaction and pressure reach certain value (100～200 ℃, 1～3atm), preparation feedback finishes.Solution is filtered, and after drying under 200～400 ℃ of temperature, depolymerization obtains the calcium sulfate crystal whiskers product.With scanning electron microscope or transmission electron microscope the calcium sulfate crystal whiskers product is detected, the result shows that the product crystalline form is fibrous, and diameter is that 1～4 μ m, length are 50～200 μ m.
(2) example 2
Add additive in embodiment 1, concrete grammar is as follows: when the reaction beginning, regulate the pH value of gypsum emulsion, make it to reach 8～12, other condition obtains the calcium sulfate crystal whiskers product with example 1.The product detected result shows that crystalline form is a ca sulphate fibre, Fibre diameter below 100nm, length-to-diameter ratio 50～1000.
Claims (5)
1. Preparation methods of gypsum whiskers method, this method is with plaster stone (CaSO
42H
2O) and water be raw material, through raw material preparation, building-up reactions, dehydrate and an operation such as refining and edulcoration, it is characterized in that selected raw material plaster stone (CaSO
42H
2O) effective content will reach more than 95, whiteness is more than 90%, being mixed with concentration by weight percentage at normal temperatures with tap water is 4～14% plaster stone slip, after mulser is fully emulsified, add and make it that chemical reaction takes place in the synthesis reactor, adding pH adjustment agent makes solution reach certain potential of hydrogen, and under the certain reaction temperature and pressure, constantly stir with certain speed, the process certain reaction time enters into later operation again.
2. according to the said Preparation methods of gypsum whiskers method of claim 1, it is characterized in that in the method that said certain reaction temperature and pressure is meant that temperature of reaction is that 100～200 ℃, reaction pressure are 1～3atm.
3. according to the said Preparation methods of gypsum whiskers method of claim 1, it is characterized in that in the method that said adding pH adjusts agent and makes solution reach certain potential of hydrogen to be meant that the pH value of solution value reaches 8～12.
4. according to the said Preparation methods of gypsum whiskers method of claim 1, it is characterized in that the said process certain reaction time is meant that reaction time range is 30～45min in the method,
5. according to the said Preparation methods of gypsum whiskers method of claim 1, it is characterized in that said constantly the stirring with certain speed is meant that stirring velocity is 400～1000rpm in the method.
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| CN100451182C (en) * | 2007-01-23 | 2009-01-14 | 东北大学 | Production of non-metallic material calcium-sulfate whiskers |
| 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 | 国家海洋局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 |
| CN101586255B (en) * | 2009-06-08 | 2011-05-04 | 安徽工业大学 | Preparation method of calcium sulphate dihydrate crystal whisker |
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| 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 |
| CN101736403B (en) * | 2009-12-14 | 2012-05-30 | 昆明理工大学 | Method for preparing calcium sulfate crystal whiskers by using impurity-containing gypsum as raw material |
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| CN104928752A (en) * | 2015-07-06 | 2015-09-23 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulphate dihydrate crystal whiskers at normal temperature and method thereof for converting calcium sulphate dihydrate crystal whiskers into anhydrous crystal whiskers at normal pressure |
| CN105401219A (en) * | 2015-12-31 | 2016-03-16 | 中国科学院青海盐湖研究所 | Normal pressure acidification method for preparing anhydrous calcium sulfate whiskers |
| CN105874013A (en) * | 2013-12-06 | 2016-08-17 | 佐治亚-太平洋石膏有限责任公司 | Calcium sulfate crystals and methods for making the same |
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| CN1337369A (en) * | 2000-08-03 | 2002-02-27 | 韩晨光 | Gypsum fiber producing process |
| CN1261624C (en) * | 2003-07-08 | 2006-06-28 | 宁夏建筑材料研究院 | Gypsum whisker, its preparation method and application |
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2004
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| CN100451182C (en) * | 2007-01-23 | 2009-01-14 | 东北大学 | Production of non-metallic material calcium-sulfate whiskers |
| 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 | 国家海洋局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 |
| CN101586255B (en) * | 2009-06-08 | 2011-05-04 | 安徽工业大学 | Preparation method of calcium sulphate dihydrate crystal whisker |
| 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 |
| CN101736403B (en) * | 2009-12-14 | 2012-05-30 | 昆明理工大学 | Method for preparing calcium sulfate crystal whiskers by using impurity-containing gypsum as raw material |
| CN102212884A (en) * | 2011-05-04 | 2011-10-12 | 上海大学 | Method for preparing calcium sulfate crystal whisker from many kinds of industrial waste residue gypsum serving as raw materials |
| CN102675919A (en) * | 2012-05-07 | 2012-09-19 | 长沙理工大学 | Preparation method for calcium sulfate whisker papermaking coating pigment |
| CN102776569A (en) * | 2012-07-09 | 2012-11-14 | 泰山医学院 | Method for preparing calcium sulfate crystal whiskers by using natural gypsum |
| CN105874013B (en) * | 2013-12-06 | 2020-07-24 | 佐治亚-太平洋石膏有限责任公司 | Calcium sulfate crystal and method for producing same |
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| CN105874013A (en) * | 2013-12-06 | 2016-08-17 | 佐治亚-太平洋石膏有限责任公司 | Calcium sulfate crystals and methods for making the same |
| CN103694717A (en) * | 2013-12-30 | 2014-04-02 | 上海浦东路桥建设股份有限公司 | Road bitumen with high heat conduction efficiency and preparation method thereof |
| CN104313726A (en) * | 2014-10-10 | 2015-01-28 | 孙红芳 | Preparation method for gypsum fibers |
| CN104928758A (en) * | 2015-05-13 | 2015-09-23 | 四川理工学院 | Mixed additives and method for producing anhydrous dead-burned type of calcium sulfate whisker |
| CN104928758B (en) * | 2015-05-13 | 2017-06-30 | 四川理工学院 | A kind of additive package and method for producing anhydrous dead roasting type calcium sulfate crystal whiskers |
| CN104911688B (en) * | 2015-06-08 | 2018-01-09 | 中国科学院青海盐湖研究所 | The preparation method of anhydrous calcium sulfate whisker |
| CN104911688A (en) * | 2015-06-08 | 2015-09-16 | 中国科学院青海盐湖研究所 | Preparation method of anhydrous calcium sulfate whisker |
| CN104928752A (en) * | 2015-07-06 | 2015-09-23 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulphate dihydrate crystal whiskers at normal temperature and method thereof for converting calcium sulphate dihydrate crystal whiskers into anhydrous crystal whiskers at normal pressure |
| CN105401219B (en) * | 2015-12-31 | 2018-03-20 | 中国科学院青海盐湖研究所 | A kind of method that normal pressure acidization prepares anhydrous calcium sulfate whisker |
| CN105401219A (en) * | 2015-12-31 | 2016-03-16 | 中国科学院青海盐湖研究所 | Normal pressure acidification method for preparing anhydrous calcium sulfate whiskers |
| CN107778618A (en) * | 2016-08-29 | 2018-03-09 | 广西金滩管业科技有限公司 | Antibacterial impact PE feed pipes and its production method |
| CN106811801A (en) * | 2017-01-24 | 2017-06-09 | 东南大学 | A kind of preparation method of modified gypsum whisker |
| CN108085740A (en) * | 2017-12-30 | 2018-05-29 | 应城市嘉鸿技术服务科技有限公司 | A kind of preparation method of anhydrous calcium sulfate whisker |
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