WO2009123097A1 - 塩基性硫酸マグネシウム粒状物及びその製造方法 - Google Patents
塩基性硫酸マグネシウム粒状物及びその製造方法 Download PDFInfo
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- WO2009123097A1 WO2009123097A1 PCT/JP2009/056472 JP2009056472W WO2009123097A1 WO 2009123097 A1 WO2009123097 A1 WO 2009123097A1 JP 2009056472 W JP2009056472 W JP 2009056472W WO 2009123097 A1 WO2009123097 A1 WO 2009123097A1
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- magnesium sulfate
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/045—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing sulfur, e.g. sulfates, thiosulfates, gypsum
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- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/40—Magnesium sulfates
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/50—Agglomerated particles
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/21—Attrition-index or crushing strength of granulates
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
- Y10T428/2982—Particulate matter [e.g., sphere, flake, etc.]
Definitions
- the present invention relates to a basic magnesium sulfate granular material that can be advantageously used as a wastewater treatment material and a method for producing the same.
- particulate magnesium sulfate such as a fiber
- a wastewater treatment material One of the uses of particulate magnesium sulfate [MgSO 4 ⁇ 5Mg (OH) 2 ⁇ 3H 2 O] such as a fiber
- Documents that disclose the use of basic magnesium sulfate as a wastewater treatment material include the following documents.
- Patent Document 1 discloses a method for removing fine particles and oil in waste water by using basic magnesium sulfate particulates composed of a plurality of fibrous basic magnesium sulfate particles.
- waste water containing fine particles and oil is brought into contact with basic magnesium sulfate particulates, whereby the fine particles and oil in the waste water are aggregated, and the aggregation of the fine particles is separated by a filter. Is described.
- Patent Document 2 discloses a basic magnesium sulfate granular material in which a plurality of fibrous basic magnesium sulfate particles are bonded to each other using a fibrous inorganic compound such as zonotolite or sepiolite or fibrillated polytetrafluoroethylene as a binder. It is disclosed. This basic magnesium sulfate granular material is said to be useful as a wastewater treatment material because of its high shape stability in running water compared to basic magnesium sulfate granular material produced without using a binder. Patent Document 2 describes that basic magnesium sulfate has an effect of adsorbing and removing silica and lead.
- Patent Document 3 as a method for removing fluorine in wastewater discharged from a desulfurization apparatus, magnesium hydroxide is used as an adsorbent of the desulfurization apparatus, and sodium hydroxide is added to the wastewater discharged from the desulfurization apparatus.
- a method for producing basic magnesium sulfate and magnesium hydroxide adsorbing fluorine is disclosed. JP-A-6-2226017 JP-A-2005-231927 JP 2003-47972 A
- the granular material composed of fibrous basic magnesium sulfate particles is an effective material for wastewater treatment because it has the effect of agglomerating fine particles and oil in wastewater and the effect of adsorbing and removing heavy metals and fluorine. is there.
- the basic magnesium sulfate granular material used as a wastewater treatment material has voids formed therein so that water can easily enter the granular material, that is, the bulk density is low, and in the water flow It is preferable that the shape stability in water is high, that is, the strength is high so that the fibrous particles do not collapse and flow out.
- an object of the present invention is to provide a basic magnesium sulfate granular material having a low bulk density and a high strength, and a method for producing the same.
- the present inventor added a predetermined amount of magnesium hydroxide, magnesium sulfate and water to a large number of fibrous basic magnesium sulfate particles to obtain a water-containing granular composition, and then at a temperature in the range of 50 to 250 ° C. It was found that by heating, basic magnesium sulfate granules having a low bulk density and a high crushing strength can be obtained, and the present invention has been completed.
- the present invention relates to fibrous basic magnesium sulfate particles, 5 to 300 parts by mass of magnesium hydroxide with respect to 100 parts by mass of the fibrous basic magnesium sulfate particles, the fibrous basic magnesium sulfate particles, and the A hydrous granular composition containing 0.1 to 200 parts by mass of magnesium sulfate with respect to 100 parts by mass of the total amount of magnesium hydroxide and having a moisture content in the range of 10 to 60% by mass is in the range of 50 to 250 ° C. It exists in the manufacturing method of the basic magnesium sulfate granular material which consists of heating at temperature for 1 hour or more.
- the preferable aspect of the manufacturing method of the basic magnesium sulfate granular material of this invention is as follows.
- the fibrous basic magnesium sulfate particles have an average length in the range of 3.0 to 200 ⁇ m, an average thickness in the range of 0.2 to 3.0 ⁇ m, and an average aspect ratio of 3 or more. Fibrous particles.
- Magnesium hydroxide is a particle having an average particle size in the range of 0.1 to 10 ⁇ m.
- Magnesium hydroxide is contained in an amount in the range of 5 to 200 parts by mass with respect to 100 parts by mass of the fibrous basic magnesium sulfate particles.
- Magnesium sulfate is contained in an amount in the range of 0.04 to 1 mol with respect to 1 mol of magnesium hydroxide.
- the fibrous basic magnesium sulfate particles and the magnesium hydroxide particles are added to 100 parts by mass of the fibrous basic magnesium sulfate particles.
- a step of obtaining a water-containing solid composition a step of forming the water-containing solid composition into a granule to obtain a water-containing granular composition, and the water-containing granular composition at a temperature in the range of 50 to 250 ° C. for 1 hour or more
- the manufacturing method of the basic magnesium sulfate granular material including the process of heating.
- the present invention further includes fibrous basic magnesium sulfate particles, magnesium hydroxide particles, and concentration containing magnesium hydroxide particles in an amount in the range of 5 to 300 parts by mass with respect to 100 parts by mass of fibrous basic magnesium sulfate particles.
- There is also a method for producing basic magnesium sulfate granules comprising a step of heating for 1 hour or more at a temperature in the range of ⁇ 250 ° C.
- the basic magnesium sulfate granules obtained by the production method of the present invention usually have a crushing strength in the range of 1.0 to 10.0 kg and a bulk density of 0.5 to 1.5 g / cm 3 . Is in range. That is, the present invention is a granular material composed of fibrous basic magnesium sulfate particles having a crushing strength in the range of 1.0 to 10.0 kg and a bulk density of 0.5 to 1.5 g / cm 3 . There are also basic magnesium sulfate granules in the range.
- a basic magnesium sulfate granule having a low bulk density and a high crushing strength can be advantageously produced industrially. Since the basic magnesium sulfate granular material of the present invention has a high crushing strength while having a low bulk density, it is useful as a wastewater treatment material.
- the method for producing the basic magnesium sulfate granular material of the present invention after adding a plurality of fibrous basic magnesium sulfate particles to a water-containing granular composition by adding magnesium hydroxide, magnesium sulfate and water in a predetermined ratio, Heat at a temperature of 50 ° C or higher.
- the fibrous basic magnesium sulfate particles used in the present invention have an average length in the range of 3.0 to 200 ⁇ m, an average thickness in the range of 0.2 to 3.0 ⁇ m, and an average aspect ratio of 3 or more.
- the fibrous particles are preferable.
- Magnesium hydroxide is preferably present in the water-containing granular composition as particles having an average particle size in the range of 0.1 to 10 ⁇ m.
- the content of magnesium hydroxide in the water-containing granular composition is generally in the range of 5 to 300 parts by mass, preferably in the range of 5 to 200 parts by mass with respect to 100 parts by mass of the fibrous basic magnesium sulfate particles. is there.
- Magnesium sulfate is preferably present in the water-containing granular composition in a dissolved state in water.
- the content of magnesium sulfate in the water-containing granular composition is generally 0.1 to 200 parts by mass, preferably 0.1 to 200 parts by mass with respect to 100 parts by mass of the total amount of fibrous basic magnesium sulfate particles and magnesium hydroxide. The amount is in the range of 120 parts by mass.
- the content of magnesium sulfate in the water-containing granular composition is preferably 0.04 mol or more, particularly 0.04 to 1 mol, with respect to 1 mol of magnesium hydroxide.
- the water-containing granular composition may further contain a fibrous inorganic compound such as zonotolite or sepiolite as a binder for the fibrous basic magnesium sulfate particles.
- a fibrous inorganic compound such as zonotolite or sepiolite as a binder for the fibrous basic magnesium sulfate particles.
- the amount of the fibrous inorganic compound is generally in the range of 1 to 40 parts by mass, preferably 5 to 30 parts by mass with respect to 100 parts by mass of the fibrous basic magnesium sulfate particles.
- the water-containing granular composition contains water in an amount such that the water content is in the range of 10 to 60% by mass.
- the water content of the water-containing granular composition is a percentage of the sample with respect to loss on drying when the sample is heated and dried at a temperature of 180 ° C. by infrared irradiation.
- the heating temperature of the water-containing granular composition is generally in the range of 50 to 250 ° C, preferably in the range of 50 to 130 ° C, particularly preferably in the range of 90 to 120 ° C.
- the heating time is generally 1 hour or longer, preferably 5 to 100 hours.
- the water-containing granular composition is, for example, a fibrous basic magnesium sulfate particle and a magnesium hydroxide particle in a magnesium sulfate aqueous solution having a concentration in the range of 1 to 40% by mass, and 100 parts by mass of the fibrous basic magnesium sulfate particle.
- the concentration of the magnesium sulfate aqueous solution used for the production of the water-containing granular composition is preferably in the range of 1 to 30% by mass, and preferably in the range of 1 to 10% by mass.
- An aqueous dispersion in which fibrous basic magnesium sulfate particles and magnesium hydroxide particles are dispersed in an aqueous magnesium sulfate solution is a method of simultaneously adding fibrous basic magnesium sulfate particles and magnesium hydroxide particles to an aqueous magnesium sulfate solution Either by adding magnesium hydroxide particles to a magnesium sulfate aqueous solution containing fibrous basic magnesium sulfate particles or by adding fibrous basic magnesium sulfate particles to a magnesium sulfate aqueous solution in which magnesium hydroxide particles are dispersed. Can be prepared. Instead of magnesium hydroxide particles, magnesium oxide particles may be used, or a part of magnesium sulfate may be precipitated as magnesium hydroxide particles using an alkali such as sodium hydroxide or ammonia.
- a method for obtaining a water-containing solid composition by dehydrating an aqueous dispersion known solid-liquid separation methods such as filtration, decantation and centrifugation can be used. Also, a method of removing water from the aqueous dispersion by heating can be used.
- a usual forming method such as an extrusion method, a compression method, or a rolling granulation method can be used.
- the water-containing granular composition also has a concentration of 1 to 40 with the magnesium hydroxide particles in an amount in the range of 5 to 300 parts by mass with respect to 100 parts by mass of the fibrous basic magnesium sulfate particles. It can manufacture by adding the magnesium sulfate aqueous solution which exists in the range of the mass%, and shape
- the amount of the magnesium sulfate aqueous solution added is such that the water content of the water-containing granular composition is in the range of 10 to 60% by mass.
- fibrous basic magnesium sulfate particles are put into a granulator that gives a rolling motion to the material to produce granules, and the magnesium hydroxide particles and magnesium sulfate aqueous solution are added to the fibrous basic magnesium sulfate particles.
- a water-containing granular composition can be produced by a method of imparting rolling motion to the resulting mixture while or after the addition.
- the magnesium hydroxide particles and the magnesium sulfate aqueous solution may be added simultaneously, or the magnesium sulfate aqueous solution may be added after the magnesium hydroxide particles are added first.
- a rolling granulating device or a stirring granulating device can be used as a granulating device for producing a granular material by giving a rolling motion to the material.
- the rolling granulator is a device that gives a rolling motion to a material by the rotation of a rotating body attached to the granulator body or the granulator.
- the agitation granulator is a granulator that gives a rolling motion to a material by agitation of a stirring blade.
- the basic magnesium sulfate granules produced as described above usually have a crushing strength in the range of 1.0 to 10.0 kg and a bulk density in the range of 0.5 to 1.5 g / cm 3 . It is in. That is, the basic magnesium sulfate granular material of the present invention has a bulk density in the range of about 22 to 65% with respect to the true density (2.3 g / cm 3 ) and a large void inside, but the crushing strength. Shows a high crushing strength in the range of 1.0 to 10.0 kg.
- the basic magnesium sulfate granular material of the present invention exhibits high crushing strength, as shown in FIG. 1, between the fibrous basic magnesium sulfate particles 1a and the fibrous basic magnesium sulfate particles 1b,
- the reaction product 2 of magnesium hydroxide and magnesium sulfate in the presence of water partially precipitates to join the fibrous basic magnesium sulfate particles 1a and the fibrous basic magnesium sulfate particles 1b. .
- the presence of this reaction product can be confirmed by an electron microscope.
- the basic magnesium sulfate granular material of the present invention is not particularly limited with respect to the particle shape, and may have any shape such as a spherical shape, a cylindrical shape, an almond shape, and a flake shape.
- the basic magnesium sulfate granular material of the present invention has a low bulk density, that is, sufficient voids in the interior, so that water easily enters the interior. Moreover, since the basic magnesium sulfate granular material of this invention has high crushing strength, its shape stability is also high in water. Therefore, the basic magnesium sulfate granular material of the present invention can be advantageously used as a wastewater treatment material.
- the moisture content of the water-containing granular composition obtained in this example was measured using an infrared moisture meter (FD-800, manufactured by Kett Scientific Laboratory) in a drying temperature of 180 ° C. and in an automatic stop mode. Further, the crushing strength, bulk density, looseness density and specific surface area of the basic magnesium sulfate granules obtained in this example were measured by the following methods.
- Example 1 To 98 kg of magnesium sulfate aqueous solution having a magnesium sulfate concentration (anhydrous conversion) of 5.0% by mass, 2.0 kg of fibrous basic magnesium sulfate particles having an average length of 20.0 ⁇ m and an average thickness of 0.5 ⁇ m were added. By stirring, an aqueous magnesium sulfate solution in which basic magnesium sulfate particles having a pH of 8.8 were dispersed was prepared.
- magnesium hydroxide fine particles (average particle size: 2.9 ⁇ m) are added, stirred, and fibrous basic magnesium sulfate particles and water are added to the magnesium sulfate aqueous solution.
- An aqueous dispersion in which magnesium oxide particles are dispersed was prepared. The pH of the obtained aqueous dispersion was 9.4.
- the aqueous dispersion was subjected to solid-liquid separation by vacuum filtration to recover a hydrated solid composition.
- the recovered water-containing solid composition was pressure dehydrated using a felt press type pressure dehydrator, and then an extrusion granulator (meet chopper, manufactured by Hiraga Kogaku Co., Ltd.) having a diameter of 2.3 mm for the face plate hole was used. It was used and granulated to obtain a cylindrical hydrous granular composition.
- the obtained cylindrical water-containing granular composition has a fibrous basic magnesium sulfate particle amount of 41.5% by mass, a magnesium hydroxide particle amount of 8.3% by mass, and a magnesium sulfate aqueous solution amount of 50.2% by mass.
- the water content was 45% by mass.
- This cylindrical water-containing granular composition is put into a box-shaped dryer and heated at a temperature of 110 ° C. for 48 hours to form cylindrical basic magnesium sulfate granules having an average diameter of 2.5 mm and an average height of 3.5 mm. I got a thing.
- FIG. 3 is a graph showing the change over time in the test force when a compressive load is applied to the basic magnesium sulfate granular material with a pressurizing tool when the crushing strength is measured.
- Example 1 A basic magnesium sulfate granule was produced in the same manner as in Example 1 except that the magnesium hydroxide fine particles were not added to the basic magnesium sulfate particle-dispersed magnesium sulfate aqueous solution.
- the obtained granular material had an average diameter of 2.5 mm and an average length of 3.5 mm.
- Table 1 shows the crushing strength, bulk density, looseness density and specific surface area of the obtained basic magnesium sulfate granules.
- This mixture was granulated using an extrusion granulator (meet chopper, manufactured by Hiraga Kogaku Co., Ltd.) having a plate hole diameter of 2.3 mm to obtain a cylindrical hydrous granular composition.
- This cylindrical water-containing granular composition was put into a box-shaped dryer and heated at a temperature of 120 ° C. for 24 hours to form a cylindrical basic magnesium sulfate having an average diameter of 2.5 mm and an average height of 3.5 mm.
- Granules were obtained.
- Table 1 shows the crushing strength, bulk density, looseness density and specific surface area of the obtained basic magnesium sulfate granules.
- Example 2 Magnesium sulfate fine particles (0.13 kg) were added to magnesium sulfate aqueous solution (2.0 kg) having a magnesium sulfate concentration (anhydride conversion) of 5.0% by mass, and stirred to obtain sulfuric acid in which magnesium hydroxide particles having a pH of 9.8 were dispersed. A magnesium aqueous solution was prepared.
- An apex granulator (manufactured by Taihei Koki Co., Ltd., stirring granulator) was charged with 1.0 kg of fibrous basic magnesium sulfate particles having an average length of 10.0 ⁇ m and an average thickness of 0.5 ⁇ m. While adding 1.32 kg of the above magnesium hydroxide particle-dispersed magnesium sulfate aqueous solution to the fibrous basic magnesium sulfate particles little by little, the resulting mixture was rolled to obtain a spherical hydrous granular composition. The obtained water-containing granular composition had a water content of 45% by mass. This water-containing granular composition was put in a box dryer and heated at a temperature of 110 ° C. for 48 hours to obtain basic magnesium sulfate granular materials.
- Example 3 A basic magnesium sulfate granule was produced in the same manner as in Example 2 except that 1.32 kg of clean water was used instead of the magnesium hydroxide particle-dispersed magnesium sulfate aqueous solution.
- Table 1 shows the crushing strength, bulk density, looseness density and specific surface area of the obtained basic magnesium sulfate granules.
- the basic magnesium sulfate granules obtained according to the method of the present invention have higher crushing strength than the basic magnesium sulfate granules obtained by the conventional method.
- FIG. 2 is an electron micrograph of basic magnesium sulfate granules produced in Example 1.
- FIG. It is a graph which shows a time-dependent change of the test force when a compressive load is applied to the basic magnesium sulfate granular material manufactured in Example 1 with the pressurizer which moves at a speed of 0.5 mm / min.
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Abstract
Description
従って、本発明は、嵩密度が低くかつ強度が高い塩基性硫酸マグネシウム粒状物及びその製造方法を提供することを目的とする。
(1)繊維状塩基性硫酸マグネシウム粒子が、平均長さが3.0~200μmの範囲にあって、平均太さが0.2~3.0μmの範囲にある、平均アスペクト比が3以上の繊維状粒子である。
(2)水酸化マグネシウムが、平均粒子径が0.1~10μmの範囲にある粒子である。
(3)水酸化マグネシウムが、該繊維状塩基性硫酸マグネシウム粒子100質量部に対して5~200質量部の範囲の量にて含まれている。
(4)硫酸マグネシウムが、水酸化マグネシウム1モルに対して、0.04~1モルの範囲の量にて含まれている。
本発明の塩基性硫酸マグネシウム粒状物は、低嵩密度でありながらも高い圧壊強度を有するため、排水処理材として有用である。
(株)島津製作所製の万能試験機オートグラフAG-1を用いて、加圧具を移動速度(クロスヘッド速度)0.5mm/分の条件で移動させて、測定対象の粒状物に圧縮荷重をかけて該粒状物に付与した力(試験力、単位:N)を経時的に測定する。試験力の経時変化から最初のピーク値を読み取り、その値を荷重(kg)に換算する。測定は5回行なって、その平均値を圧壊強度とする。なお、測定対象の粒状物が円柱状である場合は、粒状物の側面を加圧面とする。
耐火物技術協会学術振興委員会で制定された、マグネシアクリンカーのケロシン媒体のアルキメデス法による嵩密度測定方法に準じて測定する。
ホソカワミクロン(株)製のパウダーテスターを用いて、容量100cm3の容器に粒状物を充填し、容器内に充填された粒状物の質量を容器容量(100cm3)で除して算出する。
窒素吸着によるBET一点法で測定する。
硫酸マグネシウム濃度(無水物換算)5.0質量%の硫酸マグネシウム水溶液98kgに、平均長さが20.0μm、平均太さが0.5μmの繊維状塩基性硫酸マグネシウム粒子2.0kgを投入し、撹拌して、pHが8.8の塩基性硫酸マグネシウム粒子が分散された硫酸マグネシウム水溶液を調製した。この塩基性硫酸マグネシウム粒子分散硫酸マグネシウム水溶液に、水酸化マグネシウム微粒子(平均粒子径:2.9μm)0.4kgを添加し、撹拌して、硫酸マグネシウム水溶液中に繊維状塩基性硫酸マグネシウム粒子と水酸化マグネシウム粒子とが分散されている水性分散液を調製した。得られた水性分散液のpHは9.4であった。
図3は、圧壊強度の測定に際して、塩基性硫酸マグネシウム粒状物に加圧具にて圧縮荷重をかけたときの試験力の経時変化を示すグラフである。図3に示すように、試験力の最初のピーク値は22.7Nであった。従って、圧壊強度は2.3kg(=22.7/9.8)であった。
塩基性硫酸マグネシウム粒子分散硫酸マグネシウム水溶液に水酸化マグネシウム微粒子を添加しなかったこと以外は、実施例1と同じ操作を行なって、塩基性硫酸マグネシウム粒状物を製造した。得られた粒状物は、平均直径が2.5mm、平均長さが3.5mmであった。
平均長さが28μm、平均太さが0.5μmの繊維状塩基性硫酸マグネシウム粒子6kgを水194kgに分散させて調製した繊維状塩基性硫酸マグネシウム水性分散液を、真空ろ過により固液分離し、フェルトプレス式加圧脱水装置を用いて加圧脱水して、含水率50質量%の含水固体状組成物を得た。この含水固体状組成物2kgに、平均長さが3μm、平均太さが0.3μmの繊維状ゾノトライト粒子を固形分中の含有量が20質量%となるように添加して、混合した。この混合物を目板穴直径2.3mmの押出造粒装置(ミートチョッパー、(株)平賀工作所製)を用いて造粒して、円柱状含水粒状組成物を得た。この円柱状含水粒状組成物を、箱形乾燥機に入れて、120℃の温度で24時間加熱して、平均直径が2.5mm、平均高さが3.5mmの円柱状の塩基性硫酸マグネシウム粒状物を得た。
得られた塩基性硫酸マグネシウム粒状物の圧壊強度、嵩密度、緩み密度及び比表面積を表1に示す。
硫酸マグネシウム濃度(無水物換算)5.0質量%の硫酸マグネシウム水溶液2.0kgに、水酸化マグネシウム微粒子0.13kgを投入し、撹拌して、pH9.8の水酸化マグネシウム粒子が分散された硫酸マグネシウム水溶液を調製した。
水酸化マグネシウム粒子分散硫酸マグネシウム水溶液の代わりに、上水1.32kgを使用したこと以外は、実施例2と同じ操作を行なって、塩基性硫酸マグネシウム粒状物を製造した。
2 反応生成物
Claims (10)
- 繊維状塩基性硫酸マグネシウム粒子と、該繊維状塩基性硫酸マグネシウム粒子100質量部に対して5~300質量部の水酸化マグネシウムと、該繊維状塩基性硫酸マグネシウム粒子と該水酸化マグネシウムの合計量100質量部に対して0.1~200質量部の硫酸マグネシウムとを含み、含水率が10~60質量%の範囲にある含水粒状組成物を50~250℃の範囲の温度で1時間以上加熱することからなる塩基性硫酸マグネシウム粒状物の製造方法。
- 繊維状塩基性硫酸マグネシウム粒子が、平均長さが3.0~200μmの範囲にあって、平均太さが0.2~3.0μmの範囲にある、平均アスペクト比が3以上の繊維状粒子である請求項1に記載の塩基性硫酸マグネシウム粒状物の製造方法。
- 水酸化マグネシウムが、平均粒子径が0.1~10μmの範囲にある粒子である請求項1に記載の塩基性硫酸マグネシウム粒状物の製造方法。
- 水酸化マグネシウムが、該繊維状塩基性硫酸マグネシウム粒子100質量部に対して5~200質量部の範囲の量にて含まれている請求項1に記載の塩基性硫酸マグネシウム粒状物の製造方法。
- 硫酸マグネシウムが、水酸化マグネシウム1モルに対して、0.04~1モルの範囲の量にて含まれている請求項1に記載の塩基性硫酸マグネシウム粒状物の製造方法。
- 濃度が1~40質量%の範囲にある硫酸マグネシウム水溶液中に、繊維状塩基性硫酸マグネシウム粒子と水酸化マグネシウム粒子とが、該繊維状塩基性硫酸マグネシウム粒子100質量部に対して該水酸化マグネシウム粒子が5~300質量部の範囲となる割合で分散されている水性分散液を調製する工程、該水性分散液を脱水して、含水率が10~60質量%の範囲にある含水固体状組成物を得る工程、該含水固体状組成物を粒状に成形して、含水粒状組成物を得る工程、そして、含水粒状組成物を50~250℃の範囲の温度で1時間以上加熱する工程を含む塩基性硫酸マグネシウム粒状物の製造方法。
- 水酸化マグネシウム粒子を繊維状塩基性硫酸マグネシウム粒子100質量部に対して5~300質量部の範囲の量にて含む、繊維状塩基性硫酸マグネシウム粒子、水酸化マグネシウム粒子及び濃度が1~40質量%の範囲にある硫酸マグネシウム水溶液の混合物を粒状に成形して、含水率が10~60質量%の範囲にある含水粒状組成物を得る工程、そして、含水粒状組成物を50~250℃の範囲の温度で1時間以上加熱する工程を含む塩基性硫酸マグネシウム粒状物の製造方法。
- 請求項1、6、7のうちのいずれかの項に記載の方法で製造した塩基性硫酸マグネシウム粒状物であって、嵩密度が0.5~1.5g/cm3の範囲にあって、圧壊強度が1.0~10.0kgの範囲にある塩基性硫酸マグネシウム粒状物。
- 繊維状塩基性硫酸マグネシウム粒子からなる粒状物であって、嵩密度が0.5~1.5g/cm3の範囲にあって、圧壊強度が1.0~10.0kgの範囲にある塩基性硫酸マグネシウム粒状物。
- 繊維状塩基性硫酸マグネシウム粒子が、平均長さが3.0~200μmの範囲にあって、平均太さが0.2~3.0μmの範囲にある、平均アスペクト比が3以上の繊維状粒子である請求項9に記載の塩基性硫酸マグネシウム粒状物。
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KR101494611B1 (ko) * | 2013-01-24 | 2015-02-24 | 한국세라믹기술원 | 염기성 황산마그네슘 화합물의 제조방법 |
EP3110311A4 (en) | 2014-02-24 | 2017-09-27 | Medtronic Monitoring, Inc. | Separable monitoring device and method |
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JP6612481B1 (ja) * | 2018-07-26 | 2019-11-27 | 宇部マテリアルズ株式会社 | 塩基性硫酸マグネシウム粉末、塩基性硫酸マグネシウム粉末の製造方法、塩基性硫酸マグネシウム粉末を含有する樹脂組成物、マスターバッチパレット、および成形体 |
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