CN101311355A - Process for preparing calcium sulphate whiskers from ardealite - Google Patents
Process for preparing calcium sulphate whiskers from ardealite Download PDFInfo
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- CN101311355A CN101311355A CNA2008100583245A CN200810058324A CN101311355A CN 101311355 A CN101311355 A CN 101311355A CN A2008100583245 A CNA2008100583245 A CN A2008100583245A CN 200810058324 A CN200810058324 A CN 200810058324A CN 101311355 A CN101311355 A CN 101311355A
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Abstract
The invention relates to a method for preparing calcium sulphate crystal whisker by using phosphogypsum, which belongs to the technical field of phosphorous chemical preparation. Solid drogs phosphogypsum is used as raw material; after a synthetic reaction, filtering, heating and dissolving, thermal filtering and cooling crystallization for the raw material, the calcium sulphate crystal whisker product with the controllable diameter and length is prepared, the diameter of the crystal whisker is 1-4mum and the length of the crystal whisker is 50-200mum. The adoption of the solid drogs phosphogypsum for preparing the calcium sulphate crystal whisker reduces the production volume of natural plaster, saves resources, turns the waste into benefit, lowers the production cost of the calcium sulphate crystal whisker and improves added value of the product in the process of utilizing the phosphogypsum. The obtained calcium sulphate crystal whisker has excellent property, low cost and wide application.
Description
One, technical field:
The present invention relates to a kind of method of utilizing the solid slag preparing calcium sulphate whiskers from ardealite, belong to the phosphorous chemical industry preparing technical field.
Two, background technology:
Phosphogypsum is that Rock Phosphate (72Min BPL) and sulfuric acid react and the industrial residue that produces in the Wet-process Phosphoric Acid Production process, to produce 4～5 tons of phosphogypsums by the phosphoric acid that calculates 1 ton of every production, at present the quantity discharged in whole world phosphogypsum every year reaches more than 200,000,000 ton, but the utilization ratio of phosphogypsum does not surpass 10%, and the processing of phosphogypsum, disposal and comprehensive utilization have become a global difficult problem.China's phosphate fertilizer production ranks first in the world, and the phosphate fertilizer of production high density (as phosphorus ammonium, coarse whiting etc.) needs a large amount of phosphoric acid by wet processes, also can produce a large amount of phosphogypsum slags thereupon.Great majority are stored up or are toppled over, and the stacking of phosphogypsum not only takies a large amount of soils, expends a huge sum of money, and sour water leakage pollution water source, form secondary pollution.The main chemical compositions of phosphogypsum is identical with the plaster of paris, is sulphur, calcium and the gypsum resource with multiple potential use, but impurity such as the phosphorus that it contained, fluorine, organism, alkali metal constitute adverse influence to comprehensive utilization.Therefore, from the angle of the environment protection and the utilization of resources, the processing of phosphogypsum slag is extremely urgent with utilization.
At present, all phosphogypsum is decomposed a kind of important channel of system producing sulfuric acid and jointly cement both at home and abroad as the phosphogypsum comprehensive utilization, these two kinds of staple products of sulfuric acid and cement had both been obtained, and sulfuric acid can be used for this enterprise phosphoric acid production, it is under-supply to remedy sulfuric acid, can solve the outlet of phosphogypsum again, administer the pollution of phosphogypsum environment.But, big, the poor product quality of existing phosphogypsum system producing sulfuric acid and jointly cement industry investment, and its phosphogypsum decomposes to burn till in device of rotary kiln with cement clinker and finishes, because the technical problems that also exist are difficult to utilization and extention.
Whisker is meant a kind of fibrous single crystal that grows under artificial control condition, have certain length-to-diameter ratio (generally greater than 10), and normal length is 2～300 μ m, and diameter is about 0.1～10 μ m.Whisker is because its special single crystal structure, thereby has complete profile and perfect internal structure, and intensity is high, and size is trickle, is that the important matrix material of a class strengthens constituent element.
(Calcium Sulfate Whisker CSW) is crystal whisker of gypsum again to calcium sulfate crystal whiskers, is CaSO
4Fibrous single crystal, the same branch with gypsum with anhydrous, Ban Shui and two water.Calcium sulfate crystal whiskers wherein anhydrous and half water has maximum strength and higher use value, thereby its research also has bigger economic worth with application.Compare with other whiskers, it also has the characteristics that production cost is lower and toxicity is minimum except having better enhancing and modification function.
At publication number is the preparation method who discloses a kind of non-metallic material calcium-sulfate whiskers among the CN 101029415A.This method is raw material and sulfuric acid reaction with the converter slag, 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; Then the leach liquor behind converter slag and the sulfuric acid reaction is filtered, washs, obtain calcium sulfate.The calcium sulfate that obtains is mixed with clear water in solid-to-liquid ratio 0.2～0.8 ratio, adjusting the pH value with alkali (calcium oxide, magnesium oxide, lime carbonate, sour magnesium, calcium hydroxide or magnesium hydroxide) is 5～9, 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 with the suspension of calcium sulfate after the modulation in temperature, be 40min～120min time of drying, obtains calcium sulfate crystal whiskers.Adopt the rare pure and mild phosphoric acid ester of second 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.
At publication number is to disclose a kind of Preparation methods of gypsum whiskers method among the CN 1955345A.This method is by at first synthetic crystallization director, the pre-treatment of technical grade calcium oxide elder generation, put into reactor 40 ℃～60 ℃ digestion, obtain lime slurry, the gained lime slurry is warming up to 40 ℃～110 ℃ in reactor, add and the equimolar sulphuric acid soln of calcium oxide, stirred 30～60 minutes, and in the process of reaction, added crystallization director, it is fully reacted.Washing after filtration,, surface treatment and drying are able to required calcium sulfate crystal whiskers product.
At publication number is the preparation technology who discloses a kind of calcium sulfate crystal whiskers material among the CN 1699638A, this technology is mixed gypsum and water by a certain percentage, make slip, above-mentioned slip is placed autoclave, the temperature and pressure and the reaction times of control reactor, after question response was finished, drying under reduced pressure promptly got calcium sulfate crystal whiskers.
Do not see with the phosphogypsum to be the relevant report that raw material prepares calcium sulfate crystal whiskers up to now, with the phosphogypsum is that the calcium sulfate crystal whiskers that raw material prepares adds in the high molecular polymer, can strengthen many performances such as polymkeric substance mechanical property, thermotolerance, be widely used at Aeronautics and Astronautics and numerous civilian industries field; If add in the plastic, rubber, can improve tensile strength, flexural strength, spring rate and the heat-drawn wire of matrix material; Also can replace asbestos to add abrasives, material of construction, lagging material to simultaneously; Can be used as reinforcing filler and be used for industries such as polymer matrix composites, binding agent.Calcium sulfate crystal whiskers excellent property, cheap, environmental protection have wide application and market outlook.Utilize preparing calcium sulphate whiskers from ardealite, can make the solid waste phosphogypsum obtain the high-touch feature material.
Three, summary of the invention
The method that the purpose of this invention is to provide a kind of preparing calcium sulphate whiskers from ardealite, with the solid slag phosphogypsum is raw material, preparing diameter of whiskers through synthetic reaction, filtration, heating for dissolving, heat filtering, crystallisation by cooling is 1～4 μ m, length 50～200 μ m, the calcium sulfate crystal whiskers product of diameter and length controlled.
Fabricating technology route of the present invention as shown in Figure 1, it is finished according to the following steps:
(1) the raw material phosphogypsum being mixed with concentration expressed in percentage by weight is 5～15% slurries, join in the synthesis reactor, it is 7.5～12 that adding pH adjustment agent makes the potential of hydrogen of solution, controlled temperature is 90～200 ℃, evenly stir 20～30min, obtain calcium sulfate crystal whiskers first intermediates, described adjustment agent is sodium hydroxide or potassium hydroxide;
(2) calcium sulfate crystal whiskers first intermediates are filtered, after the filtration weight in wet base per-cent is 30～45% filter residue, be calcium sulfate crystal whiskers second intermediates;
(3) heating for dissolving: it is 5%～20% slurries that second intermediates are mixed with weight percent concentration, controlled temperature is 100～200 ℃, evenly stir 20～30min, in the process that stirs, add the additive magnesium nitrate powder (Mg (NO of 0.15～0.2 times of raw material weight simultaneously
3)
2.6H
2O) as the crystalline form growth substance, the diameter and the length of control calcium sulfate crystal whiskers obtain calcium sulfate crystal whiskers the 3rd intermediates;
(4) the 3rd intermediates temperature remain on 80～150 ℃ and carry out heat filtering, and heat filtering gained filtrate is calcium sulfate crystal whiskers the 4th intermediates of water ratio 30～45%;
(5) crystallisation by cooling: the 4th intermediates are at room temperature cooled off, separate out crystal, treat that crystal all separates out, (in the water behind the no flocculence object), stop going up cooling, the crystal that obtains is calcium sulfate crystal whiskers, cools off available cold water, frozen water or icy salt solution etc., with the gained calcium sulfate crystal whiskers temperature is 150～310 ℃ dry 1～2 hour down, make water content less than 0.3% calcium sulfate crystal whiskers product.
Major advantage of the present invention has:
(1) calcium sulfate crystal whiskers product diameter, length is even, quality is high;
(2) use the solid waste preparing calcium sulphate whiskers from ardealite, reduced the produced quantity of the plaster of paris, saved resource, reduced the production cost of calcium sulfate crystal whiskers simultaneously, improved phosphogypsum and utilized value-added content of product in the process;
(3) this technology does not have strict restriction for the composition of raw material phosphogypsum, and is applied widely, condition is wide;
(4) production technique environmentally safe, the calcium sulfate crystal whiskers excellent property of gained, with low cost, have multiple purposes widely.
Four, Fig. 1 is the preparing calcium sulphate whiskers from ardealite process flow sheet.
Five, embodiment
Embodiment 1: raw material phosphogypsum main chemical compositions weight percent/be: CaO 35.36%, SO
247.12%, Fe
2O
33.01%, Al
2O
32.05%, P
2O
51.20%, F 0.06%, SiO
211.20%.It is 10% phosphogypsum slurries that phosphogypsum is mixed with weight percent concentration, joins in the synthesis reactor, adds pH and adjusts agent sodium hydroxide, make the potential of hydrogen of solution be adjusted into 9, controlled temperature is 95 ℃, evenly stirs 25min, obtains calcium sulfate crystal whiskers first intermediates; Utilize box filter that first intermediates of preparing are previously filtered, the weight in wet base per-cent that filters the gained filter residue is 32%, and this is calcium sulfate crystal whiskers second intermediates; It is 15% slurries that second intermediates are mixed with weight percent concentration, when temperature is 120 ℃, evenly stirs 25min, adds 0.15 times of MgNO of raw material weight simultaneously in the process that stirs
3As the crystalline form growth substance, the diameter and the length of control calcium sulfate crystal whiskers obtain calcium sulfate crystal whiskers the 3rd intermediates.Is to carry out heat filtering under 100 ℃ with the 3rd intermediates in temperature, obtaining weight in wet base per-cent is that 36% filtrate is calcium sulfate crystal whiskers the 4th intermediates, cool off with frozen water, after treating that crystal is all separated out, in temperature is under 150 ℃ of following dryings dry 1.5 hours, promptly obtains the calcium sulfate crystal whiskers product.With scanning electron microscope product is detected, the result shows that the diameter of calcium sulfate crystal whiskers is that 2～4 μ m and length are 100～200 μ m.This calcium sulfate crystal whiskers adopts stearic acid as surface-modifying agent, carries out adding in the plastic, rubber after the surface modification, can improve tensile strength, flexural strength and the spring rate of matrix material.
Embodiment 2: raw material phosphogypsum main chemical compositions/% is: CaO=37%, SO
2=50.17%, Fe
2O
3=0.1%, Al
2O
3=0.59%, P
2O
5=1.01%, F=0.01%, SiO
2=11.12%.It is 12% phosphogypsum slurries that phosphogypsum is mixed with weight percent concentration, join in the synthesis reactor, add pH and adjust agent potassium hydroxide, make the potential of hydrogen of solution be adjusted into 10, and when temperature is 95～100 ℃, evenly stir 30min, obtain calcium sulfate crystal whiskers first intermediates; Utilize centrifugal filter that first intermediates of preparing are previously filtered, the weight in wet base per-cent that filters the gained filter residue is 43%, is calcium sulfate crystal whiskers second intermediates; It is 16% slurries that these second intermediates are mixed with weight percent concentration, when temperature is 140 ℃, evenly stirs 30min, adds 0.2 times of MgNO of raw material weight simultaneously in the process that stirs
3As the crystalline form growth substance, the diameter and the length of control calcium sulfate crystal whiskers obtain calcium sulfate crystal whiskers the 3rd intermediates.The 3rd intermediates are carried out heat filtering when temperature is 100 ℃ after, obtaining weight in wet base per-cent is that 35% filtrate is calcium sulfate crystal whiskers the 4th intermediates, cool off with frozen water, after treating that crystal is all separated out, in temperature is under 200 ℃ of following dryings dry 1.5 hours, promptly obtains the calcium sulfate crystal whiskers product.With scanning electron microscope product is detected, the result shows that the diameter of calcium sulfate crystal whiskers is that 1～4 μ m and length are 50～150 μ m.This calcium sulfate crystal whiskers adopts blast furnace slag as surface-modifying agent, carry out surface modification after, add in the high molecular polymer, can strengthen polymkeric substance mechanical property and thermotolerance.
Claims (2)
1, a kind of method of preparing calcium sulphate whiskers from ardealite, it is characterized in that: it is finished according to the following steps:
1) the raw material phosphogypsum being mixed with concentration expressed in percentage by weight is 5～15% slurries, join in the synthesis reactor, it is 7.5～12 that adding pH adjustment agent makes the potential of hydrogen of solution, and controlled temperature is 90～200 ℃, evenly stir 20～30min, obtain calcium sulfate crystal whiskers first intermediates;
2) calcium sulfate crystal whiskers first intermediates are filtered, after the filtration weight in wet base per-cent is 30～45% filter residue, be calcium sulfate crystal whiskers second intermediates;
3) heating for dissolving: it is 5%～20% slurries that second intermediates are mixed with weight percent concentration, controlled temperature is 100～200 ℃, evenly stir 20～30min, in the process that stirs, add the additive magnesium nitrate powder of 0.15～0.2 times of raw material weight simultaneously as the crystalline form growth substance, the diameter and the length of control calcium sulfate crystal whiskers obtain calcium sulfate crystal whiskers the 3rd intermediates;
4) the 3rd intermediates temperature remains on 80～150 ℃ and carries out heat filtering, and heat filtering gained filtrate is calcium sulfate crystal whiskers the 4th intermediates of water ratio 30～45%;
5) the 4th intermediates are at room temperature cooled off, separate out crystal, treat that crystal all separates out, the crystal that obtains is calcium sulfate crystal whiskers, with the gained calcium sulfate crystal whiskers temperature is 150～310 ℃ dry 1～2 hour down, make water content less than 0.3% calcium sulfate crystal whiskers product.
2, the method for preparing calcium sulphate whiskers from ardealite according to claim 1 is characterized in that: described adjustment agent is sodium hydroxide or potassium hydroxide.
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| CN115305574A (en) * | 2022-07-21 | 2022-11-08 | 武汉理工大学 | Method for rapidly preparing crystal whisker by using phosphogypsum and saline water |
| CN115305574B (en) * | 2022-07-21 | 2023-09-19 | 武汉理工大学 | Method for rapidly preparing whisker by using phosphogypsum and saline |
| WO2024021234A1 (en) * | 2022-07-28 | 2024-02-01 | 广东邦普循环科技有限公司 | Method for preparing calcium sulfate whiskers by means of phosphogypsum purification |
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