WO2001047809A1 - Processus de traitement d'aluminosilicate de sodium - Google Patents

Processus de traitement d'aluminosilicate de sodium Download PDF

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Publication number
WO2001047809A1
WO2001047809A1 PCT/JP2000/009443 JP0009443W WO0147809A1 WO 2001047809 A1 WO2001047809 A1 WO 2001047809A1 JP 0009443 W JP0009443 W JP 0009443W WO 0147809 A1 WO0147809 A1 WO 0147809A1
Authority
WO
WIPO (PCT)
Prior art keywords
sodium
sodium aluminosilicate
aluminosilicate
elution
calcium compound
Prior art date
Application number
PCT/JP2000/009443
Other languages
English (en)
Japanese (ja)
Inventor
Yasuo Kawai
Isao Ishikawa
Yoshiyuki Takenaka
Hideya Saito
Mineo Nozaki
Original Assignee
Showa Denko K. K.
Tsukishima Kikai Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Showa Denko K. K., Tsukishima Kikai Co., Ltd. filed Critical Showa Denko K. K.
Priority to AU22318/01A priority Critical patent/AU2231801A/en
Priority to JP2001549292A priority patent/JP4480317B2/ja
Publication of WO2001047809A1 publication Critical patent/WO2001047809A1/fr

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/24—Cements from oil shales, residues or waste other than slag
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/20—Silicates
    • C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
    • C01B39/026—After-treatment
    • 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

Definitions

  • the present invention relates to a method for treating sodium aluminosilicate.
  • sodium aluminosilicate which is currently discarded or not effectively used, such as red mud and soda light generated during the production of alumina and aluminum, zeolite used in various applications, Alternatively, by separating sodium contained in naturally occurring zeolite and sodalite, the recovery and utilization of sodium and the removal of sodium-removed residue from semite are performed. It can be effectively used as a raw material for packaging. Background art
  • a typical example of sodium aluminosilicate is red hydroxide produced as a by-product of the production of aluminum hydroxide and alumina. About 800 kg of this red mud is produced for 1 ton of aluminum. Red mud, A 1 2 O 3, S i O, the aluminosilicate sodium and F e 2 ⁇ 3 consisting of N a 2 O as a main component, and the other, T i 0 2, quartz, alumina Contains several percent of hydrates and lime compounds. Possible uses include cement raw materials and steelmaking raw materials. However, it has been considered difficult to use cement raw materials because it contains a large amount of Na and steel raw materials contain a large amount of A1. Therefore, red mud has been discarded as industrial waste without being used.
  • zeolite used in various applications. Zeolite is generally used as a catalyst supporting a metal catalyst and a noble metal catalyst, and for ion exchange. Some are recycled and used in most cases After removing harmful and useful components, the carrier zeolite is discarded as industrial waste.
  • a main object of the present invention is to recover a useful component of Na among the components contained in sodium aluminosilicate and further reduce the Na concentration of a substance discharged as a residue.
  • the purpose is to propose a treatment method that can be effectively used as a cement raw material. Disclosure of the invention
  • the present invention recovers the Na component at a higher rate than various types of sodium aluminosilicate in order to effectively use the sodium aluminosilicate that has been discarded or not used without being used effectively at present.
  • a method for treating sodium aluminosilicate to obtain a useful substance having a very low content characterized by the following preferred features. (1) A calcium compound as a simple substance or a mixture of calcium oxide, calcium carbonate, calcium hydroxide, calcium sulfate, or the like, or a mixture containing them, particularly preferably calcium oxide, is added to sodium aluminosilicate. Add and mix.
  • the amount of the calcium compound added is such that the sodium component in the sodium aluminosilicate is expressed as Na 2 O, and the silicon component is expressed as a molar ratio of Ca ON a 2 O when expressed as Si 0 2. Or (preferably “and”) C a ⁇ ZS i 0 2 force; ⁇ 5, preferably 2.0 ⁇ 4.0.
  • the particle size of the sodium aluminosilicate and the calcium compound to be added is not particularly specified, but includes a particle size of 1 ⁇ m to 300 ⁇ m, more preferably a particle size of 60 ⁇ m or less. Things are good.
  • the mixture may be either dry or wet, but is more preferably wet.
  • the mixture of (1) is subjected to a heat treatment at 800 to 140 ° C., more preferably 100 to 135 ° C., using a heater such as a kiln.
  • the mixture to be heat-treated may be in the form of a powder or a pellet, and the form is not particularly limited.
  • the heat treatment time is from 5 minutes to 180 minutes, more preferably from 20 to 80 minutes.
  • the high-temperature exhaust gas generated by the heater generates steam in a boiler, etc., recovers waste heat, and recovers energy.
  • the heat-treated product obtained in (2) is eluted with water (or an aqueous solution) to elute and recover sodium.
  • the amount of water (or aqueous solution) at this time is 1 to 30 times by weight, more preferably 10 to 20 times by weight, of the heat-treated product.
  • the elution temperature is 50 ° C or higher, more preferably 70 ° C or higher.
  • the elution time is between 10 and 120 minutes, more preferably between 60 and 90 minutes.
  • FIG. 1 shows an embodiment of the process of the present invention.
  • FIG. 2 shows an example (1) of an apparatus configuration for performing the process of the present invention.
  • FIG. 3 shows an example (part 2) of an apparatus configuration for performing the process of the present invention.
  • FIG. 4 shows an example (part 3) of an apparatus configuration for performing the process of the present invention.
  • the sodium aluminosilicate according to the present invention includes sodalite discharged in the production of aluminum hydroxide, aluminum, and metallic aluminum. Zeolites used in various applications, natural and synthetic zeolites and sodalites, etc. Either way.
  • the soda light emitted in the production of aluminum is generally Na 2 O power; 18 to 25 weight 0 /. , A 1 2 O 3 power s 3 1 ⁇ 3 8 weight 0 I, S i O 2 2 8-3 5 wt%, impurities such as F e 2 O 3 contains 5 wt% or less.
  • Zeorai bets expressed in ionic formula, C a O ⁇ A 1 2 0 3 ⁇ 4 S i 0 2 -. 6 5 H 2 ⁇ , N a 2 O - A 1 2 0 3 ⁇ 2 S i 0 2 - . 4 5 H 2 0, N a 2 O ⁇ A 1 2 0 3 - 2 5 S i 0 2 ⁇ 6 H 2 O.
  • This sodium aluminosilicate may be obtained as red mud containing iron in bauxite treatment, but in the present invention, sodium aluminosilicate separated from iron is preferred.
  • Preferred correct aluminosilicate soda in the present invention aluminosilicate soda 9 0 wt% or more, good Ri rather preferably 9 5 those containing by weight% or more, or 1 0 weight iron content in the F e 2 ⁇ 3 %, More preferably less than 5% by weight.
  • a method of obtaining sodium aluminosilicate separated from iron in bauxite treatment is known. However, there is no particular problem if sodium aluminosilicate contains iron and other metal components. However, the more the soda light, the less the energy consumption per soda light.
  • the calcium compound calcium oxide, calcium carbonate, calcium hydroxide, calcium sulfate, and the like, and in some cases, a mixture thereof can be used. Calcium oxide is preferred.
  • the calcium compound and the sodium aluminosilicate react to convert the soda component into a compound that can be dissolved in water. it can.
  • the product that can be eluted is probably a product containing sodium aluminate.
  • the amount of the calcium compound to be added is such that when the sodium component in the sodium aluminosilicate is represented by Na 2 O and the silicon component is represented by Si 0 2 , the molar ratio is C a OZN a 2 O or Z and C a OZ S i 0 2 is typically 1 or more, properly favored properly is preferred 1-5, yo Ri may range from 2-4. If these ratios are less than 1, it is not possible to make a compound capable of sufficiently eluting the soda content in the sodium aluminosilicate. If these ratios are too large, compounds that are difficult to elute may be formed, and the elution rate of soda may decrease.
  • the sodium aluminosilicate and the calcium compound are ground to reduce the particle size.
  • the soda elution rate can be increased.
  • the sodium aluminosilicate and the calcium compound may be mixed in a dry state, but C a ⁇ partially dissolves as C a (OH) 2, and the Na and C a of the sodalite in the liquid phase before firing. It is preferable that water is added and mixed in a wet state, since the mixture may undergo a substitution reaction.When mixed in a wet state, the mixture can be pelletized and pelletized. Is preferred. By forming pellets, generation of dust during firing is suppressed, and transfer is facilitated. When pelletizing, since the reactivity depends on the particle size of the original particles, it is desirable that the original particles have the above-mentioned particle size.
  • the mixture of the sodium aluminosilicate and the calcium compound is generally heated at a temperature of 800 to 140 ° C, particularly preferably 100 to 135 ° C.
  • the heating temperature has a large effect on the soda elution rate after heating. It is considered that a heating temperature within a certain range is required to generate compounds that can be easily eluted.
  • the heating atmosphere may be in the air.
  • the heating time is not particularly limited, but is generally 5 to 180 minutes, and is preferably 20 to 80 minutes. Is preferred. Heating rate 'Although not limited, generally 10 to 30 ° C / min may be used. Cooling may be either rapid cooling or slow cooling.
  • the heating device is not limited, but kilns and the like are industrially advantageous (a substance produced by this heat treatment may be referred to as a heat-treated product).
  • the heat-treated product is preferably ground to facilitate elution.
  • Elution is performed with water or an aqueous solution.
  • the amount of water or aqueous solution is not particularly limited, but is preferably 1 to 30 times by weight, more preferably 10 to 20 times by weight of the heat-treated product. Elution can be promoted by using warm water. It is generally at least 50 ° C, preferably at least 70 ° C.
  • the elution time is not particularly limited, but may be 5 to 120 minutes, preferably 60 to 90 minutes.
  • sodium aluminosilicate and a calcium compound are mixed, heated, and soda is eluted, so that the amount of soda in the eluted residue can be extremely reduced. It is possible.
  • the residual soda content can be reduced to 1% or less, further to 0.6% or less, 0.1% or less, and particularly to 0.01% or less.
  • the solid of sodium recovered from sodium which is mainly composed of calcium silicate, can be used as a cement raw material.
  • the recovery (extraction) rate of more than 95%, more preferably more than 99%, especially more than 99.9% is calculated as the recovery rate of soda in sodium aluminosilicate. It can be achieved.
  • a mixing device 1 for example, a double kneader. Mix O well.
  • This mixture is supplied from line 13 to heating device 2, for example, a kiln, and is calcined at 100 ° C. to 135 ° C.
  • the calcined product is sent through line 14 to a cooling device 3, for example, a rotary cooler or a steel belt cooler, where it is cooled, and then, through line 15, a crushing device 4, for example, a hammer. It is supplied to a mill and pulverized.
  • the pulverized material pulverized by the pulverizing device 4 in the firing step is supplied to the elution device 5 via the pipe 16 together with the water (or aqueous solution) from the pipe 17 and is stirred at 50 ° C. Elution is performed at ⁇ 100 ° C.
  • the slurry of the elution device 5 is extracted from the pipe 18 and separated into solid and liquid by a solid-liquid separation device 6, for example, a horizontal belt finoletter or a rotary drum finoletter.
  • the filtrate containing the useful component sodium is withdrawn through line 20 and reused.
  • the separated cake is washed by the washing water supplied from the pipe 19, and discharged from the pipe 21.
  • This sodium recovery residue is mainly composed of calcium and silica. Since the rubber content is less than 1%, it is effectively used as a cement raw material. Also, the washing filtrate at this time is extracted from the pipe 20 and reused.
  • FIGS. 2 to 4 disassemble and show a configuration example of the apparatus more specifically for performing the process of the present invention.
  • sodalite is supplied to a mixer 31 via a sodalite storage tank 32, and a Ca ⁇ storage tank 33, a Ca ⁇ pulverizer 34, and a CaO quantitative feeder 3 are provided.
  • the mixture is fed into the kiln 37 via the kiln charging device 36, the mixture is injected into the kiln 37 via the kiln charging device 36 Fired at temperature.
  • the calcined product is cooled by a cooler 38, it is pulverized by a crusher / pulverizer 39, and then subjected to elution treatment with warm water in an elution tank 40.
  • the slurry subjected to the elution treatment is separated into a filtrate and a cake by a filter 41, and the filtrate passes through a filtrate tank 42, passes through an evaporative concentrator 43, and is used in an alumina treatment process such as a Bayer method. Is done.
  • the cake after filtration is passed through a cake receiving tank 44, a dryer 45, and a drying cake receiving tank 46, and is used as a cement raw material. 47 is a bug fino letter.
  • Table 1 shows the analytical values of sodalite obtained from the desiliconization process added to the Bayer method for the production of aluminum hydroxide and alumina.
  • This soda light, CaO having a particle size of 53 ⁇ xm or less, and water in such an amount that the total water content of the mixture becomes 40% are put into a mixing device and mixed.
  • the mixture is calcined in a kiln at 1200 ° C. for a residence time of 30 minutes, and then cooled. And cooled, and then pulverized by a pulverizer.
  • the pulverized product was put into an elution tank, water was added at 20 times the weight of the calcined product (pulverized product), and the mixture was mixed well at 90 ° C for 60 minutes to perform elution. Next, the elution slurry was supplied to a filter to perform solid-liquid separation, and the separated cake was thoroughly washed with water.
  • the obtained recovered liquid and cake were chemically analyzed for the sodium component concentration, and the recovery ratio of the sodium component and the remaining sodium concentration in the cake were determined. As a result, a high sodium recovery rate of 99.9% was obtained, and the sodium concentration of the insoluble residue was also very low at 0.01% dry%.
  • a useful material that can be used as a raw material was obtained. Soda light analysis value
  • the pulverized product was put into an elution tank, water was added at 20 times the weight of the calcined product (pulverized product), and the mixture was mixed well at 90 ° C for 60 minutes to perform elution. Next, the elution slurry was supplied to a filter to perform solid-liquid separation, and the separated cake was thoroughly washed with water.
  • the obtained recovered liquid and cake were chemically analyzed for the sodium component concentration, and the recovery rate of the sodium component and the sodium remaining concentration in the cake were determined. I asked. As a result, the recovery rate of sodium was 22.5%, and the sodium concentration of the insoluble residue was 8.81 dry%.
  • the pulverized product was put into an elution tank, water was added at 20 times the weight of the calcined product (pulverized product), and the mixture was mixed well at 90 ° C for 60 minutes to perform elution. Next, the elution slurry was supplied to a filter to perform solid-liquid separation, and the separated cake was thoroughly washed with water.
  • the sodium concentration of the obtained recovered liquid and cake was chemically analyzed to determine the sodium component recovery rate and the sodium concentration remaining in the cake. As a result, the sodium recovery was 61.8%, and the sodium concentration of the insoluble residue was 4.33 dry 0 /. Met.
  • Table 2 shows the analysis values of synthetic zeolite 4A.
  • the zeolite and CaO are charged into a mixing device and mixed.
  • This mixture was calcined in a kiln at 1200 ° C. for a residence time of 60 minutes, then put into a cooling device, cooled, and then pulverized by a pulverizer.
  • the pulverized product was put into an elution tank, water was added at 20 times the weight of the calcined product (pulverized product), and the mixture was mixed well at 90 ° C for 60 minutes to perform elution.
  • the elution slurry was supplied to a filter to perform solid-liquid separation, and the separated cake was thoroughly washed with water.
  • the obtained recovered liquid and The sodium component concentration in the cake was chemically analyzed to determine the sodium component recovery rate and the residual sodium concentration in the cake. As a result, a high sodium recovery of 93.4% was obtained, and the sodium concentration of the insoluble residue was extremely low at 0.66 dry%.
  • Useful materials that can be used as cement raw materials were obtained.
  • Table 2 Analytical values of zeolite (used synthetic zeolite 4A) As described above, according to the present invention, the following effects can be obtained.
  • sodium aluminosilicate which is currently discarded or not effectively used, such as red mud and soda light generated during the production of alumina and aluminum, zeolite used in various applications, Alternatively, by separating sodium contained in naturally occurring zeolite and sodalite, sodium can be recovered and sodium-removed residue can be cemented. It can be effectively used as a raw material.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Structural Engineering (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

La présente invention concerne un processus de traitement d'aluminosilicate de sodium qui consiste à ajouter un composé de calcium à un aluminosilicate de sodium, à chauffer le mélange de l'aluminosilicate de sodium et du composés de calcium qui en résulte, à soumettre ce mélange chauffé à un traitement par élution avec de l'eau ou une solution aqueuse, de façon à solubiliser et éluer d'autres composants de sodium dans l'aluminosilicate de sodium, et à récupérer ces composant de sodium, ce précédé fournissant en même temps un produit utile dont le contenu en sodium autre que l'aluminosilicate de sodium est considérablement réduit. Ce processus permet de récupérer presque complètement de l'aluminosilicate de sodium les autres composants de sodium, et également une production d'un résidu qui possède un contenu de sodium autre que l'aluminosilicate de sodium de 1 % ou moins et qui peut donc être utilisé efficacement. On peut améliorer le pourcentage de l'élution susmentionnée en optimisant les conditions de chauffage et d'élution.
PCT/JP2000/009443 1999-12-28 2000-12-28 Processus de traitement d'aluminosilicate de sodium WO2001047809A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU22318/01A AU2231801A (en) 1999-12-28 2000-12-28 Process for treating sodium aluminosilicate
JP2001549292A JP4480317B2 (ja) 1999-12-28 2000-12-28 アルミノ珪酸ソーダの処理方法

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP37546799 1999-12-28
JP11/375467 1999-12-28

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WO2001047809A1 true WO2001047809A1 (fr) 2001-07-05

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU753833B2 (en) * 1999-12-28 2002-10-31 Showa Denko Kabushiki Kaisha Process for treating bauxite
JP2007261834A (ja) * 2006-03-27 2007-10-11 Kimura Chem Plants Co Ltd ゼオライトの製造方法および製造装置
CN111072035A (zh) * 2020-01-16 2020-04-28 刘文治 一种焚烧含硅灰渣的资源化处理生产无钠硅溶胶的成套设备

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5051834A (fr) * 1973-09-14 1975-05-08
JPH05238727A (ja) * 1992-02-24 1993-09-17 Showa Denko Kk 改良アルミナ製造方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5051834A (fr) * 1973-09-14 1975-05-08
JPH05238727A (ja) * 1992-02-24 1993-09-17 Showa Denko Kk 改良アルミナ製造方法

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
KAZUO AKAISHI: "Sekidei no riyou ni kansuru saikin no kenkyu doukou", KEIKINZOKU, vol. 26, no. 3, 1976, pages 150 - 163, XP002944146 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
AU753833B2 (en) * 1999-12-28 2002-10-31 Showa Denko Kabushiki Kaisha Process for treating bauxite
JP2007261834A (ja) * 2006-03-27 2007-10-11 Kimura Chem Plants Co Ltd ゼオライトの製造方法および製造装置
JP4520957B2 (ja) * 2006-03-27 2010-08-11 木村化工機株式会社 ゼオライトの製造方法および製造装置
CN111072035A (zh) * 2020-01-16 2020-04-28 刘文治 一种焚烧含硅灰渣的资源化处理生产无钠硅溶胶的成套设备
CN111072035B (zh) * 2020-01-16 2023-08-29 刘文治 一种焚烧含硅灰渣的资源化处理生产无钠硅溶胶的成套设备

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JP4480317B2 (ja) 2010-06-16

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