CN101029415A - Production of non-metallic material calcium-sulfate whiskers - Google Patents
Production of non-metallic material calcium-sulfate whiskers Download PDFInfo
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- CN101029415A CN101029415A CN 200710010129 CN200710010129A CN101029415A CN 101029415 A CN101029415 A CN 101029415A CN 200710010129 CN200710010129 CN 200710010129 CN 200710010129 A CN200710010129 A CN 200710010129A CN 101029415 A CN101029415 A CN 101029415A
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- calcium sulfate
- calcium
- converter slag
- whiskers
- crystal whiskers
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Abstract
Production of non-metallic calcium sulfate whiskers is carried out by taking converter slag as raw materials, grinding, leaching out sulfuric acid, filtering to obtain calcium sulfate suspended solution, synthesizing by high-temperature crystallizing method, separating and drying to obtain the final product. The purity is above 98%. It's cheap, has better quality and short process flow path. It can be used as filler, friction material, building material or thermal-insulating material and used to substitute glass fiber.
Description
Technical field
The present invention relates to the comprehensive utilization of trade waste, be specifically related to the non-metallic material processing technique field, particularly utilize converter slag to prepare the method for calcium sulfate crystal whiskers.
Background technology
Increase year by year along with output of steel, solid waste increases year by year, converter slag is exactly wherein a kind of, and quantity discharged is generally 10%～15% of crude steel output, because calcium contents is higher in the converter slag, there is powder phenomenon-tion, restrict it and use, the range of application of converter current slag is narrower, and is low value-added product, in Environmental awareness enhanced today gradually, strengthen the research of converter slag reutilization technology has been become hot subject.
The treatment technology of converter current slag mainly contains several: reclaim the iron and steel scrap in the converter slag; Converter slag is as agglomerate flux; Converter slag returns slag as steel-making; Converter slag is as hot metal pretreatment flux; Utilize converter slag to produce cement; Converter slag after treatment is used to pave the way and produce material of construction; Converter slag is as the water quality cleansing agent in contaminated waters; With converter slag production abrasive blasting material.But aforesaid method does not all reach the effective utilization to converter slag.
Whisker is meant the certain length-to-diameter ratio shape like fibrous material that has with the growth of monocrystalline form, because the height-oriented structure of whisker, not only make it have high strength, high-modulus and high elongation rate, and has light,, magnetic, dielectric, conduction, the superconduction performance, thereby as the agent of high performance composite remodeling, more and more widely be used for automobile, aerospace, chemical industry, metallurgical, national defence, machinery, electric, boats and ships, the oil numerous areas, calcium sulfate crystal whiskers is meant the fibrous single crystal of half water or anhydrous calciumsulphate, it is a kind of excellent property, cheap new function material, can be used for resin, rubber, coating, make toughener or functional type filler in the papermaking, can be used for friction again, insulation and fire retardant material, very vast potential for future development is arranged, utilize converter slag to prepare calcium sulfate crystal whiskers, not only raw material sources are extensive, and can reduce the pollution of converter slag to surrounding environment.About the prior art of calcium sulfate crystal whiskers, produce the following method that mainly contains at present:
At first 200410050288.X adopts Hydrothermal Preparation technology with the gypsum for the feedstock production calcium sulfate crystal whiskers, it is a synthetic under alkaline condition, the present invention can be in slant acidity, synthesize under neutrality or the slight alkalinity condition, preparation a wider range, in traditional preparation method, mainly contain two kinds of methods of hot method of hydraulic pressure and normal pressure acidization, the hot method of hydraulic pressure is massfraction to be added in the water autoclave less than 2% dihydrate gypsum suspension handle, depress at saturation steam, dihydrate gypsum becomes tiny acicular semi-hydrated gypsum, again through the stable crystal formation processing, obtain the sulfate hemihydrate calcium pyroborate, this method production cost height, application is restricted.The normal pressure acidization is meant that at a certain temperature high density dihydrate gypsum suspension can be transformed into needle-like or fibrous sulfate hemihydrate calcium pyroborate in acidic solution, and equipment corrosion is serious, also has environmental pollution.
Be the feedstock production calcium sulfate crystal whiskers with the halogen slag in addition, this method is a raw material with the halogen slag of sea salt bittern after milk of lime is handled, and control saltwater brine pH value is 7.6～8.0, filters, and adds the industrial waste acid dissolving, stirs, and regulates pH value to 2～3, and heated solution is to boiling.Be that the adularescent crystal is separated out after the cooling, examine under a microscope to elongated fibrous, but experimental procedure be numerous and diverse, be difficult for industrialization.
Summary of the invention
In order to overcome the defective that prior art exists, purpose of the present invention provides a kind of preparation method of non-metallic material calcium-sulfate whiskers, mainly utilize converter slag to mix and produce non-metallic material calcium-sulfate whiskers, to reach the purpose that alleviates environmental pollution, makes rational use of resources with sulfuric acid.
Concrete technology of the present invention comprises:
(1) acidolysis: with the converter slag is raw material and sulfuric acid reaction, and the converter slag granularity is 0.04～0.09mm, and sulfuric acid concentration is 10%～30%, and add-on is 4～7 times of converter slag weight, and the reaction times is 40～120min;
(2) separate: the leach liquor behind converter slag and the sulfuric acid reaction is filtered, washs, obtain calcium sulfate;
(3) size mixing: the calcium sulfate that obtains is mixed with clear water in the ratio of solid-to-liquid ratio 0.2～0.g, and adjusting the pH value with alkali (calcium oxide, magnesium oxide, lime carbonate, magnesiumcarbonate, calcium hydroxide or magnesium hydroxide) is 5～9;
(4) high temperature crystallization: the suspension of calcium sulfate after will modulating is that 120 ℃～200 ℃, pressure are that 0.3～1MPa and mixing speed are controlled to be under 50 commentaries on classics/min～900 commentaries on classics/min conditions in temperature, and insulation 40min～480min filters, washing;
(5) drying: the calcium sulfate crystal whiskers after will washing is that be 40min～120min time of drying under 100 ℃～150 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers.
(6) cover with paint, lacquer, colour wash, etc.: adopt polyvinyl alcohol and phosphoric acid ester to carry out surface modification, dispersion calcium sulfate crystal whiskers, the consumption of properties-correcting agent is 0.5%～2%, finally obtains the calcium sulfate crystal whiskers product.
Wherein converter slag composition and weight percent are:
Converter slag composition SiO
2CaO MgO Al
2O
3Fe
2O
3Other
Weight percent 6～14 42～50 4～12 1～6 21～29 2～5
In the converter slag composition: other are S, P, F and Na.
The calcium sulfate crystal whiskers density of the inventive method preparation is 2.9g/cm
3, aerated density is 0.1～0.5g/cm
3, length is 10 μ m～240 μ m, and diameter is 50nm～5 μ m, and fusing point is 1450 ℃, and tensile strength is 20GPa, and tensile modulus is 172GPa, and refractive index is 1.58, water-soluble (22 ℃)≤0.12%.
The present invention has following advantage:
Utilize ferrous metallurgy waste-converter slag to be raw material, solved the pollution of converter slag effectively surrounding environment; Adopt the high temperature crystallization legal system to be equipped with calcium sulfate crystal whiskers, technical process is short, and production cost is low.
Description of drawings
Accompanying drawing 1 is the process flow sheet that the present invention prepares calcium sulfate crystal whiskers
Embodiment
The preparation method of a kind of non-metallic material calcium-sulfate whiskers of the present invention, embodiment is described in detail in conjunction with the embodiments.
Embodiment 1
Choose: the converter slag 40g that with the granularity is 0.074mm is raw material (converter slag composition such as table 1) and 10% sulfuric acid 240g reaction, and temperature of reaction is 50 ℃, and the reaction times is 40min; Separate after filtration, liquid phase is used to prepare mixtures such as ferric sulfate and sal epsom, and solid phase is the calcium sulfate that contains silicon-dioxide; Calcium sulfate is mixed with clear water in 5: 1 ratio in solid-to-liquid ratio, and adjusting the pH value with calcium oxide is 5; Suspension of calcium sulfate after the modulation is rendered in the reactor, is that 120 ℃, pressure are that 0.3MPa and mixing speed are controlled to be under the condition of 50 commentariess on classics/min in temperature, and insulation 480min filters, washs; With the calcium sulfate crystal whiskers after the washing is that soaking time is 120min under 100 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers; Adopt polyvinyl alcohol that calcium sulfate crystal whiskers is carried out surface modification, dispersion, the consumption of properties-correcting agent is 0.5%, finally obtains the anhydrous calcium sulfate whisker product; The length of whisker is 10～30 μ m, and diameter is 50nm～100nm, and wherein liquid phase can prepare red iron oxide and sal epsom product.
Table 1 converter slag composition
Converter slag composition SiO
2CaO MgO Al
2O
3Fe
2O
3Other
Weight percent 10.24 48.62 6.89 1.62 27.23 5.4
Wherein: other are S, P, F and Na
Embodiment 2
Choose: the converter slag 40g that with the granularity is 0.09mm is raw material (converter slag composition such as table 2) and 15% sulfuric acid 160g reaction, and temperature of reaction is 90 ℃, and the reaction times is 40min; Separate after filtration, liquid phase is used to prepare ferric oxide, and solid phase is a calcium sulfate, and calcium sulfate is mixed with clear water in 0.4 ratio in solid-to-liquid ratio, and adjusting the pH value with calcium oxide is 6; Suspension of calcium sulfate after the modulation is rendered in the reactor, is that 150 ℃, pressure are that 0.6MPa and mixing speed are controlled to be under the condition of 100 commentariess on classics/min in temperature, and insulation 240min filters, washs; With the calcium sulfate crystal whiskers after the washing is that soaking time is 120min under 100 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers; Adopt polyvinyl alcohol that calcium sulfate crystal whiskers is carried out surface modification, dispersion, the consumption of properties-correcting agent is 0.5%, finally obtains the anhydrous calcium sulfate whisker product; The length of whisker is 40～90 μ m, and diameter is 80nm～160nm.Wherein liquid phase can prepare red iron oxide and sal epsom product, and wherein liquid phase can prepare red iron oxide and sal epsom product.
Table 2 converter slag composition
Converter slag composition SiO
2CaO MgO Al
2O
3Fe
2O
3Other
Weight percent 9.594 9.73 8.24 2.48 25.26 4.7
Wherein: other are S, P, F and Na
Embodiment 3
Choose: the converter slag 40g that with the granularity is 0.074mm is raw material (converter slag composition such as table 1) and 20% sulfuric acid 160g reaction, and temperature of reaction is 70 ℃, and the reaction times is 40min; Separate after filtration, liquid phase is used to prepare ferric oxide, and solid phase is a calcium sulfate, and calcium sulfate is mixed with clear water in 0.6 ratio in solid-to-liquid ratio, and adjusting the pH value with calcium oxide is 7; Suspension of calcium sulfate after the modulation is rendered in the reactor, is that 190 ℃, pressure are that 0.8MPa and mixing speed are controlled to be under the condition of 200 commentariess on classics/min in temperature, and insulation 300min filters, washs; With the calcium sulfate crystal whiskers after the washing is that soaking time is 60min under 140 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers; Adopt polyvinyl alcohol that calcium sulfate crystal whiskers is carried out surface modification, dispersion, the consumption of properties-correcting agent is 0.5%, finally obtains the anhydrous calcium sulfate whisker product; The length of whisker is 80～130 μ m, and diameter is 320nm～430nm, and wherein liquid phase can prepare red iron oxide and sal epsom product.
Embodiment 4
Choose: the converter slag 40g that with the granularity is 0.05mm is raw material (converter slag composition such as table 1) and 10% sulfuric acid 160g reaction, and temperature of reaction is 50 ℃, and the reaction times is 60min; Separate after filtration, liquid phase is used to prepare ferric oxide, and solid phase is a calcium sulfate; Calcium sulfate is mixed with clear water in 0.5 ratio in solid-to-liquid ratio, and adjusting the pH value with magnesium oxide is 8; Suspension of calcium sulfate after the modulation is rendered in the reactor, is that 120 ℃, pressure are that 0.3MPa and mixing speed are controlled to be under the condition of 400 commentariess on classics/min in temperature, and insulation 120min filters, washs; With the calcium sulfate crystal whiskers after the washing is that soaking time is 80min under 120 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers; Adopt phosphoric acid ester that calcium sulfate crystal whiskers is carried out surface modification, dispersion, the consumption of properties-correcting agent is 1%, finally obtains the anhydrous calcium sulfate whisker product; The length of whisker is 120～160 μ m, and diameter is 1 μ m～1.5 μ m, and wherein liquid phase can prepare red iron oxide and sal epsom product.
Embodiment 5
Choose: the converter slag 40g that with the granularity is 0.04mm is raw material (converter slag composition such as table 2) and 10% sulfuric acid 240g reaction, and temperature of reaction is 90 ℃, and the reaction times is 90min; Separate after filtration, liquid phase is used to prepare ferric oxide, and solid phase is a calcium sulfate; Calcium sulfate is mixed with clear water in 0.8 ratio in solid-to-liquid ratio, and adjusting the pH value with magnesium oxide is 9; Suspension of calcium sulfate after the modulation is rendered in the reactor, is that 160 ℃, pressure are that 0.7MPa and mixing speed are controlled to be under the condition of 700 commentariess on classics/min in temperature, and insulation 60min filters, washs; With the calcium sulfate crystal whiskers after the washing is that soaking time is 60min under 140 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers; Adopt phosphoric acid ester that calcium sulfate crystal whiskers is carried out surface modification, dispersion, the consumption of properties-correcting agent is 1%, finally obtains the anhydrous calcium sulfate whisker product; The length of whisker is 150～220 μ m, and diameter is 3 μ m～4 μ m, and wherein liquid phase can prepare red iron oxide and sal epsom product.
Claims (3)
1, a kind of preparation method of non-metallic material calcium-sulfate whiskers is characterized in that this preparation technology's method comprises:
(1) acidolysis: with the converter slag is raw material and sulfuric acid reaction, and the converter slag granularity is 0.04～0.09mm, and sulfuric acid concentration is 10%～30%, and add-on is 4～7 times of converter slag weight, and the reaction times is 40～120min;
(2) separate: the leach liquor behind converter slag and the sulfuric acid reaction is filtered, washs, obtain calcium sulfate;
(3) size mixing: the calcium sulfate that obtains is mixed with clear water in the ratio of solid-to-liquid ratio 0.2～0.8, and adjusting the pH value with alkali is 5～9;
(4) high temperature crystallization: the suspension of calcium sulfate after will modulating is that 120 ℃～200 ℃, pressure are that 0.3～1MPa and mixing speed are controlled to be under 50 commentaries on classics/min～900 commentaries on classics/min conditions in temperature, and insulation 40min～480min filters, washing;
(5) drying: the calcium sulfate crystal whiskers after will washing is that be 40min～120min time of drying under 100 ℃～150 ℃ the condition in temperature, obtains calcium sulfate crystal whiskers;
(6) cover with paint, lacquer, colour wash, etc.: adopt polyvinyl alcohol and phosphoric acid ester to carry out surface modification, dispersion calcium sulfate crystal whiskers, the consumption of properties-correcting agent is 0.5%～2%, finally obtains the calcium sulfate crystal whiskers product.
2, by the preparation method of the described non-metallic material calcium-sulfate whiskers of claim 1, it is characterized in that sizing mixing with alkali is calcium oxide, magnesium oxide, lime carbonate, magnesiumcarbonate, calcium hydroxide or magnesium hydroxide.
3, by the preparation method of the described non-metallic material calcium-sulfate whiskers of claim 1, it is characterized in that the composition of used converter slag is as follows by weight percentage:
SiO
2CaO MgO Al
2O
3Fe
2O
3Other
6～14 42～50 4～12 1～6 21～29 2～5 other be S, P, F and Na.
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|---|---|---|---|
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| CN100451182C CN100451182C (en) | 2009-01-14 |
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| CN101230483B (en) * | 2007-11-05 | 2010-06-09 | 安徽工业大学 | Method for preparing gypsum whisker by calcium citrate |
| CN102002756A (en) * | 2010-11-16 | 2011-04-06 | 东北大学 | Method of preparing calcium sulfate whisker by using agglomerate fume desulfurized by-products |
| CN102584122A (en) * | 2012-02-15 | 2012-07-18 | 江苏省一夫新材料科技有限公司 | Building heat preservation mortar |
| CN102618931A (en) * | 2012-04-06 | 2012-08-01 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN103422171A (en) * | 2013-05-13 | 2013-12-04 | 福建省万旗非金属材料有限公司 | Method for preparing calcium sulfate whiskers through waste residue generated in production process of calcium carbonate |
| CN103510151A (en) * | 2013-08-30 | 2014-01-15 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulfate whiskers from dolomite |
| CN103952765A (en) * | 2014-04-30 | 2014-07-30 | 江南大学 | Preparation method of conductive calcium sulfate whisker |
| CN104499040A (en) * | 2014-12-05 | 2015-04-08 | 上海宝冶钢渣综合开发实业有限公司 | Method for preparing gypsum whisker |
| CN104651944A (en) * | 2015-02-12 | 2015-05-27 | 湘潭大学 | Preparation method of calcium-sulfate-based calcium sulfate crystal whisker |
| CN104692443A (en) * | 2015-03-24 | 2015-06-10 | 枣庄市泰瑞精细化工有限公司 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
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| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
| CN106498500A (en) * | 2016-10-26 | 2017-03-15 | 四川理工学院 | A kind of method for preparing calcium sulfate crystal whiskers using non-hardening magnesia rich slags |
| CN108950674A (en) * | 2018-07-24 | 2018-12-07 | 北京科技大学 | A method of half water, anhydrous calcium sulfate whisker are prepared with one step of hydro-thermal method |
| US10280288B2 (en) | 2013-12-06 | 2019-05-07 | Georgia-Pacific Gypsum Llc | Calcium sulfate crystals and methods for making the same |
| CN110924220A (en) * | 2019-12-02 | 2020-03-27 | 上海大学 | Preparation method of bagasse fiber paper enhanced by high-strength calcium sulfate whiskers |
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| CN113830814A (en) * | 2021-09-16 | 2021-12-24 | 浙江钙宝新材料有限公司 | Method for preparing calcium sulfate nano-rods from industrial solid waste gypsum |
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| CN1261624C (en) * | 2003-07-08 | 2006-06-28 | 宁夏建筑材料研究院 | Gypsum whisker, its preparation method and application |
| CN100334264C (en) * | 2004-08-20 | 2007-08-29 | 东北大学 | Process for preparing calcium sulfate whisker |
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| CN101230483B (en) * | 2007-11-05 | 2010-06-09 | 安徽工业大学 | Method for preparing gypsum whisker by calcium citrate |
| CN102002756A (en) * | 2010-11-16 | 2011-04-06 | 东北大学 | Method of preparing calcium sulfate whisker by using agglomerate fume desulfurized by-products |
| CN102002756B (en) * | 2010-11-16 | 2013-03-20 | 东北大学 | Method of preparing calcium sulfate whisker by using sinter fume desulfurized by-products |
| CN102584122A (en) * | 2012-02-15 | 2012-07-18 | 江苏省一夫新材料科技有限公司 | Building heat preservation mortar |
| CN102618931B (en) * | 2012-04-06 | 2015-04-22 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN102618931A (en) * | 2012-04-06 | 2012-08-01 | 江苏省范群干燥设备厂有限公司 | Method for preparing calcium sulfate whiskers |
| CN103422171A (en) * | 2013-05-13 | 2013-12-04 | 福建省万旗非金属材料有限公司 | Method for preparing calcium sulfate whiskers through waste residue generated in production process of calcium carbonate |
| CN103422171B (en) * | 2013-05-13 | 2015-11-11 | 福建省万旗非金属材料有限公司 | The waste residue of calcium carbonate production process is utilized to prepare the method for calcium sulfate crystal whiskers |
| CN103510151A (en) * | 2013-08-30 | 2014-01-15 | 宁远县隆翔新型材料科技有限公司 | Method for preparing calcium sulfate whiskers from dolomite |
| US10280288B2 (en) | 2013-12-06 | 2019-05-07 | Georgia-Pacific Gypsum Llc | Calcium sulfate crystals and methods for making the same |
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| CN103952765A (en) * | 2014-04-30 | 2014-07-30 | 江南大学 | Preparation method of conductive calcium sulfate whisker |
| CN104499040B (en) * | 2014-12-05 | 2017-06-30 | 上海宝冶钢渣综合开发实业有限公司 | A kind of method for preparing crystal whisker of gypsum |
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| CN104651944A (en) * | 2015-02-12 | 2015-05-27 | 湘潭大学 | Preparation method of calcium-sulfate-based calcium sulfate crystal whisker |
| CN104651944B (en) * | 2015-02-12 | 2017-04-05 | 湘潭大学 | A kind of preparation method of the heavy metal absorbent based on calcium sulfate crystal whiskers |
| CN104692443A (en) * | 2015-03-24 | 2015-06-10 | 枣庄市泰瑞精细化工有限公司 | Manufacturing method using 1,5 naphthalene disulfonic acid reactive mother solution to prepare calcium sulfate |
| CN106241849A (en) * | 2016-06-27 | 2016-12-21 | 枣庄市泰瑞精细化工有限公司 | A kind of method utilizing the waste water producing naphthalenedisulfonic acid to prepare gypsum for cement |
| CN106498500B (en) * | 2016-10-26 | 2019-01-08 | 四川理工学院 | A method of calcium sulfate crystal whiskers are prepared using non-hardening magnesia rich slags |
| CN106498500A (en) * | 2016-10-26 | 2017-03-15 | 四川理工学院 | A kind of method for preparing calcium sulfate crystal whiskers using non-hardening magnesia rich slags |
| CN108950674A (en) * | 2018-07-24 | 2018-12-07 | 北京科技大学 | A method of half water, anhydrous calcium sulfate whisker are prepared with one step of hydro-thermal method |
| CN110924220B (en) * | 2019-12-02 | 2022-07-08 | 上海大学 | Preparation method of bagasse fiber paper enhanced by high-strength calcium sulfate whiskers |
| CN110924220A (en) * | 2019-12-02 | 2020-03-27 | 上海大学 | Preparation method of bagasse fiber paper enhanced by high-strength calcium sulfate whiskers |
| WO2021116742A1 (en) * | 2019-12-13 | 2021-06-17 | Scarab Chile Spa | Method for obtaining an alkaline earth metal compound |
| CN113830814A (en) * | 2021-09-16 | 2021-12-24 | 浙江钙宝新材料有限公司 | Method for preparing calcium sulfate nano-rods from industrial solid waste gypsum |
| CN114538840A (en) * | 2022-03-19 | 2022-05-27 | 青岛惠城环保科技股份有限公司 | Preparation method of high-strength anti-freezing foam concrete with in-situ generated whiskers |
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