WO2021065481A1 - 吸着材 - Google Patents

吸着材 Download PDF

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Publication number
WO2021065481A1
WO2021065481A1 PCT/JP2020/034898 JP2020034898W WO2021065481A1 WO 2021065481 A1 WO2021065481 A1 WO 2021065481A1 JP 2020034898 W JP2020034898 W JP 2020034898W WO 2021065481 A1 WO2021065481 A1 WO 2021065481A1
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Prior art keywords
adsorbent
cerium oxide
surface area
specific surface
oxide particles
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PCT/JP2020/034898
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English (en)
French (fr)
Japanese (ja)
Inventor
浩之 梶田
敦 黒崎
和也 木下
純一 伊東
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Mitsui Kinzoku Co Ltd
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Mitsui Mining and Smelting Co Ltd
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Priority to JP2021550573A priority Critical patent/JPWO2021065481A1/ja
Publication of WO2021065481A1 publication Critical patent/WO2021065481A1/ja
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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
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
    • 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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • 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

Definitions

  • the present invention relates to an adsorbent capable of effectively adsorbing anions contained in wastewater.
  • Anions such as fluorine ions are contained in wastewater from factories such as the electronics industry, glass processing industry, and etching processing industry.
  • Japanese wastewater standards stipulate the permissible concentration of each anionic substance as a water quality standard, for example, in the case of fluorine ions, the fluorine concentration is less than 8 mg / L.
  • Patent Document 1 discloses a fluorine adsorbent composed of a polymer resin and a rare earth element-containing oxide having a crystallite diameter of 50 to 200 ⁇ and a heat loss of 0.1 to 5% by weight.
  • Patent Document 2 discloses an adsorbent composed of a molded product containing cerium oxide particles having an average particle size of 1 to 15 ⁇ m and a crystallite size of 40 to 200 ⁇ and a binder resin.
  • Patent Document 3 discloses an adsorbent composed of a porous molded body containing an organic polymer resin and an inorganic ion adsorbent and having a most frequent pore diameter of 0.08 to 0.70 ⁇ m measured by a mercury porosimeter. ing.
  • the present invention focuses on the excellent adsorption performance of rare earth element oxides, especially cerium oxide, and can remove anions in water more effectively with respect to an adsorbent containing cerium oxide particles and binder resin. It is intended to provide an adsorbent.
  • the present invention is an adsorbent containing cerium oxide particles and a binder resin, wherein the most frequent pore diameter measured by a mercury porosimeter is less than 80 nm, and the total pore specific surface area measured by a mercury porosimeter is 10 m 2 /.
  • the adsorbent proposed by the present invention has a feature that the mode pore diameter is extremely small and the specific surface area of all pores is large, whereby anions in water can be adsorbed more effectively. it can.
  • This Adsorbent A molded product containing cerium oxide particles (referred to as “cerium oxide particles”) and a binder resin (referred to as “this binder resin”) as an adsorbent (referred to as “the present adsorbent") according to an example of the present invention.
  • This binder resin a binder resin as an adsorbent (referred to as “the present adsorbent) according to an example of the present invention.
  • the adsorbent made of the above will be described.
  • the cerium oxide particles used as this adsorbent are materials with excellent chemical resistance. By using such a material as an adsorbent, the durability against wastewater is improved, and the adsorptivity can be maintained for a long period of time.
  • the shape of the adsorbent can be formed into any shape. For example, it can be formed into a spherical shape, an elliptical spherical shape, a prismatic shape, a prismatic shape, a plate shape, a scale shape, a rod shape, a needle shape, an indefinite shape, or other shapes.
  • the shape of the adsorbent can be observed with an electron microscope (for example, a magnification of 20 to 100 times).
  • the mode adsorbent preferably has a mode pore diameter of less than 80 nm, more preferably 50 nm or less, further preferably 15 nm or less, and 10 nm or less. It is particularly preferable to have it.
  • the mode pore diameter is preferably 3 nm or more.
  • the mode pore diameter defined by the present invention shall be measured with a mercury porosimeter.
  • the most frequent pore diameter of the adsorbent is the diameter of the pores existing on the surface of the cerium oxide particles and the diameter of the pores generated when the adsorbent is molded, in other words, the diameter of the gap between the cerium oxide particles. Consists of the sum of. In any of the pores, the smaller the pore diameter, the stronger the adsorbent that has entered the pores receives the potential for interaction with the pore wall, and thus the more efficient the anions in the wastewater. It can be adsorbed well and exchanged with OH- ions on the surface of the adsorbent.
  • Total pore specific surface area This adsorbent, from the viewpoint of exhibiting a more excellent adsorption properties, it is preferred total pore specific surface area measured by a mercury porosimeter is 10 m 2 / g or more and preferably 50 m 2 / g or more, 100 m 2 among them / It is more preferably g or more. On the other hand, from the viewpoint of maintaining the strength as an adsorbent, the total pore specific surface area is preferably 200 m 2 / g or less.
  • the present adsorbent has a feature that the most frequent pore diameter is small and the total pore specific surface area is large, so that the pores having a small diameter are provided in a wide surface area. As a result, since the present adsorbent has many adsorption points, the exchange probability between the anion and the OH- ion existing on the surface of the adsorbent is high, and the anion adsorption performance is high.
  • the total pore volume of the present adsorbent is preferably 0.01 ml / g or more, more preferably 0.2 ml / g or more, as measured by a mercury porosimeter. , 0.5 ml / g or more is particularly preferable.
  • the total pore volume is preferably 10 ml / g or less.
  • the measurement by the mercury porosimeter specified in the present invention shall be carried out in the range where the pore diameter is 3 nm or more and 10,000 nm or less.
  • this adsorbent preferably has a BET specific surface area of 90 m 2 / g or more, particularly 110 m 2 / g or more, and particularly 150 m 2 / g or more. preferable.
  • the BET specific surface area is preferably 300 m 2 / g or less, and more preferably 200 m 2 / g or less. preferable.
  • the most frequent pore diameter, total pore specific surface area, total pore volume, and BET specific surface area as described above are designed by appropriately adjusting the method for producing the cerium oxide particles to be used, the molding conditions for the adsorbent, and the like. be able to. However, it is not limited to them.
  • the ratio of the total pore specific surface area to the BET specific surface area is preferably 0.1 or more, particularly 0.4 or more, and further 0.5 or more. Is more preferable. On the other hand, from the viewpoint of maintaining the strength of the present adsorbent, it is preferably less than 1.0.
  • the adsorption performance is exhibited by the water containing the adsorbent diffusing into the pores of the adsorbent and exchanging ions with the OH-ions present on the inner surface of the pores. Therefore, the higher the total pore specific surface area / BET specific surface area, that is, the larger the ratio of the surface area in the pores, the higher the adsorption efficiency of anions. In addition to this, the smaller the diameter of the pores, the stronger the adsorbent that has entered the pores receives the potential for interaction with the pore walls, so it can be considered that the adsorption efficiency of anions is high. ..
  • the present adsorbent preferably has a porosity of 40% or more, more preferably 60% or more, and more preferably 70% or more.
  • the porosity is preferably 90% or less, and more preferably 80% or less.
  • the porosity of the adsorbent can be determined by the following formula (1) using a parameter related to the density obtained by measuring with a mercury porosimeter.
  • Porosity (%) (1- (B / A)) x 100 ... Equation (1)
  • A represents "Apparent (skeletal) Density” obtained by the analysis software attached to the measuring device
  • B represents "Bulk Density at 0.0035 MPa”.
  • cerium oxide content From the viewpoint of exhibiting more excellent adsorptivity in the present adsorbent, the content of cerium oxide is preferably 90% by mass or more, and more preferably 95% by mass or more.
  • the content of cerium oxide particles contained in the adsorbent is measured as follows. As in the examples described later, when it is recognized that the amount of cerium oxide as a raw material and the amount of cerium oxide in the adsorbent are the same from the viewpoint of the method for producing the adsorbent, the amount of cerium oxide used as the raw material is used as the present material. It can be the content of cerium oxide in the adsorbent. On the other hand, if there is a possibility that the amount of cerium oxide as a raw material and the amount of cerium oxide in the adsorbent are different from the viewpoint of the manufacturing method, or if the manufacturing method is unknown, the measurement is performed by, for example, the following method. can do.
  • the mass of the adsorbent before and after heating can be measured, and the content of cerium oxide particles contained in the adsorbent can be calculated by the following formula.
  • Content of cerium oxide particles (% by mass) (W / W 0 ) x 100 (In the above formula, W 0 represents the mass (g) of the adsorbent before the heat treatment, and W represents the mass (g) of the ash after removing the binder resin component.)
  • the particle shape of the cerium oxide particles is arbitrary.
  • spherical shape, elliptical spherical shape, prismatic shape, pyramidal shape, plate shape, scale shape, rod shape, needle shape, indefinite shape, and other shapes can be mentioned.
  • the shape of the cerium oxide particles can be observed with an electron microscope (for example, a magnification of 1,000 to 100,000 times).
  • the cerium oxide particles preferably have a mode pore diameter of 1,000 nm or less, particularly preferably 750 nm or less, as measured by a mercury porosimeter.
  • the most frequent pore diameter of the cerium oxide particles is presumed to be the diameter of the pores existing on the surface of the cerium oxide particles.
  • the cerium oxide particles preferably have a total pore specific surface area of 10 m 2 / g or more, particularly preferably 50 m 2 / g or more, as measured by a mercury porosimeter. ..
  • the total pore specific surface area is preferably 100 m 2 / g or less.
  • the cerium oxide particles preferably have a total pore volume of 0.5 ml / g or more as measured by a mercury porosimeter.
  • the cerium oxide particles preferably have a BET specific surface area of 100 m 2 / g or more, and more preferably 200 m 2 / g or more.
  • the BET specific surface area is preferably 400 m 2 / g or less.
  • the ratio of the BET specific surface area of the adsorbent to the BET specific surface area of the cerium oxide particles is preferably 0.1 or more, and more preferably 0.5 or more, from the viewpoint of exhibiting more excellent adsorptivity. More preferred.
  • This binder resin has a role of binding cerium oxide particles to each other and maintaining the strength of the molded product.
  • the binder resin can be used without particular limitation as long as it can bind cerium oxide particles to each other.
  • resins include polysulfone-based polymers, polyvinylidene-fluorinated polymers, polyvinylidene chloride-based polymers, acrylonitrile-based polymers, acrylic acid ester-based polymers, polyamide-based polymers, polyimide-based polymers, and cellulose-based polymers. it can.
  • a resin that is hard to elute into water and has no biodegradability from this point of view, acrylic acid ester-based polymers, polyacrylonitrile polymers, polysulfone polymers, polyvinylidene fluoride polymers and the like are preferable.
  • the content of the binder resin is preferably 10% by mass or less, and more preferably 5% by mass or less, from the viewpoint of sufficiently exhibiting the adsorption performance of the adsorbent while binding the cerium oxide particles to each other.
  • cerium oxide particles are manufactured by a wet synthesis method carried out under temperature conditions of room temperature or lower, and the cerium oxide particles and binder resin are molded by an extrusion granulation method at a temperature of 100 ° C. or lower.
  • the cerium oxide particles are produced by a method for producing the present adsorbent or a dry synthesis method carried out under a temperature condition of 180 ° C. or lower, and the cerium oxide particles and the binder resin are extruded at a temperature of 100 ° C. or lower.
  • a method of producing the present adsorbent by molding with the above can be mentioned.
  • the present adsorbent can be produced under a temperature condition of 180 ° C. or lower from the production of the cerium oxide particles to the molding of the present adsorbent. Therefore, a molded body having desired pore characteristics can be produced. Can be done.
  • the manufacturing method of this adsorbent is not limited to these manufacturing methods.
  • the wet synthesis method it is preferable to produce the cerium oxide particles by carrying out the wet synthesis method under a temperature condition of room temperature or lower.
  • the specific surface area of the cerium oxide particles can be considerably increased as compared with the method of coprecipitating cerium nitrate with ammonia, for example.
  • the specific surface area of the particle powder becomes smaller as the particles grow, and the surface area becomes smaller. Therefore, it is preferable not to apply heat as much as possible.
  • the reaction can proceed at room temperature or lower, so that the specific surface area of the cerium oxide particles can be increased.
  • cerium oxide particles are produced by adopting the dry synthesis method
  • the cerium oxide particles are obtained by atomizing cerium carbonate as a raw material by wet pulverization and then carrying out the dry synthesis method under a temperature condition of 180 ° C. or lower. It is preferable to manufacture.
  • cerium carbonate is heated to form cerium oxide, if it is heated at a high temperature, the pores on the surface of the cerium oxide particles become large due to the vaporization of carbon dioxide gas. Therefore, in the present invention, by pulverizing cerium carbonate with a ball mill or the like, cerium carbonate can be converted into cerium oxide even by heating at a low temperature of 180 ° C. or lower, and the pores on the surface of the cerium oxide particles can be made small and the number can be reduced. You can do a lot.
  • the particle shape of cerium carbonate as a raw material may be any shape.
  • plate-shaped, rod-shaped, needle-shaped, granular and the like can be mentioned.
  • Examples of the means for wet pulverization of cerium carbonate include ball mill pulverization using zirconia balls and the like as a medium at a rotation speed of 100 rpm to 300 rpm, and bead mill pulverization.
  • Heating after wet pulverization is preferably performed at 180 ° C. or lower, and more preferably 160 ° C. or lower. On the other hand, it is preferable to carry out at 120 ° C. or higher.
  • the heating atmosphere is preferably the atmosphere.
  • ⁇ Molding method> The cerium oxide particles prepared as described above, the binder resin, and a plasticizer, if necessary, are added and kneaded, and this is extruded and granulated at a temperature of 100 ° C. or lower for molding. Is preferable. According to such a production method, since the production of the cerium oxide particles to the molding of the present adsorbent can be performed at a temperature of 180 ° C. or lower, a molded product having desired pore characteristics can be produced. However, the molding method of this adsorbent is not limited to this manufacturing method.
  • a method for mixing the cerium oxide particles and the binder resin known means can be applied without particular limitation.
  • a kneader, a mixer, a high-speed stirrer, or the like can be applied.
  • a plasticizer may be added for the purpose of imparting fluidity, shape retention, and the like.
  • plasticizer examples include water-soluble polymers.
  • cellulose ethers such as methyl cellulose, polyvinyl alcohol, polyvinyl alcohol, starch and the like can be mentioned.
  • the above-mentioned plasticizers can be used alone or in admixture of two or more. Further, if necessary, a generally used dispersant or the like may be appropriately added.
  • a mixture of cerium oxide particles and a binder resin it is preferable to supply a mixture of cerium oxide particles and a binder resin to an extrusion granulator to form a predetermined shape. It is preferable that the granulated product obtained by extrusion granulation is formed into a desired size by using a granulator, a classifier, or the like, if necessary.
  • This adsorbent can be suitably used as an adsorbent for anions existing in water, for example.
  • a column filled with this adsorbent can be used to adsorb various anions existing in water.
  • the anion include fluorine ion, boron ion, iodic acid ion, arsenate ion, phosphate ion, antimonate ion and the like.
  • the column is a tubular container provided with solid-liquid separating means such as a perforated plate or a mesh at least one of the lower part and the upper part so that the adsorbent does not flow out.
  • the material of the column is not particularly limited, and examples thereof include stainless steel, FRP (reinforced plastic containing glass fiber), glass, and various plastics.
  • the inner surface of the column may be lined with rubber or fluororesin in consideration of acid resistance.
  • All values related to the logarithmic differential void volume distribution are the measured values of the mercury intrusion porosimeter or the values calculated from the measured values.
  • the pores targeted by the present invention are only open pores (pores communicating with the outside), and closed pores (independent pores) are not included in the subject.
  • the surface tension of mercury is known, and the contact angle shows a unique value for each device. Therefore, the pore diameter (total pore volume diameter) can be calculated from the pressure of the injected mercury. Actually, it can be actually measured with an autopore IV9520 (minimum measurable hole diameter of 3 nm) manufactured by Shimadzu Corporation.
  • the "most frequent pore diameter” measured by the mercury intrusion porosimeter is the pore diameter with the highest pore volume frequency in the logarithmic differential pore volume distribution (chart) measured by the mercury intrusion porosimeter, in other words, the highest frequency. It is the pore diameter with the highest pore volume frequency at the high peak.
  • the above-mentioned "pore volume frequency” means a frequency representing the total volume of open pores corresponding to the total pore volume diameter, and the pores corresponding to the amount of change (dlogD) in the pore diameter (log). It is a value (dv / dlogD) expressed using the amount of change in volume (dv), and has a unit of volume (for example, cc / g) per unit mass.
  • ⁇ Logarithmic differential void volume distribution measurement test> To measure the specific surface area volume distribution, use a mercury intrusion porosimeter (manufactured by Shimadzu Corporation, Autopore IV9520: minimum measurable pore size 3 nm) to measure each of the cerium oxide particles and the adsorbent under the following conditions and procedures. The most frequent pore diameter, the total pore specific surface area, the BET specific surface area, and the total pore volume of the particles are determined, and the most frequent pore diameter, the total pore specific surface area, the BET specific surface area, and the total pore specific surface area / BET of the adsorbent are obtained. The specific surface area, total pore volume and porosity were determined and shown in the table.
  • Measurement condition Measurement environment: Room temperature Measurement cell: Sample chamber volume 3 cm 3 , press-fit volume 0.39 cm 3 Measuring range: From 0.0048 MPa to 413.6854 MPa. Measurement points: 136 points (points are carved so that they are evenly spaced when the pore diameter is taken logarithmically) Press-fit volume: Adjusted so as to be 25% or more and 80% or less.
  • SSA BET Specific Surface Area
  • the BET specific surface area (SSA) of the cerium oxide particles and the adsorbent was measured by the BET 1-point method using a specific surface area measuring device (Macsorb HM Model-1201) manufactured by Mountech. At that time, a mixed gas of helium as a carrier gas and nitrogen as an adsorbent gas was used.
  • Example 1 Water is added to cerium carbonate particle powder having a plate-like particle shape at a mass ratio of 1: 1 and used at room temperature (25 ° C.) for 8 hours using a ball mill (diameter 3 mm zirconia balls, rotation speed 200 rpm). Wet pulverized. The pulverized cerium carbonate particle powder was dried in the air at 60 ° C. for 24 hours using a dryer, and then calcined in the air at 180 ° C. for 12 hours in a firing furnace to obtain cerium oxide. The mode pore diameter of the obtained cerium oxide particles was 487 nm.
  • the kneaded product was extruded at room temperature (25 ° C.) on a screen having a mesh size of 0.6 mm using an extrusion granulator (disc pelleter PV-5S / 11-200D type, manufactured by Dalton), and then extruded.
  • the granulated product was obtained by performing a granulation treatment with a granulator (Malmerizer-QJ-230T-2 type, manufactured by Dalton Co., Ltd.).
  • the granulated product obtained as described above was dried with hot air at 100 ° C. for 10 minutes using a dryer (fluid dryer MGD80 type, manufactured by Dalton) to obtain an adsorbent (sample). ..
  • cerium oxide particles were bound to each other via a binder resin, and micropores were formed between the sintered bodies.
  • Example 2 cerium oxide particles and an adsorbent (sample) were obtained in the same manner as in Example 1 except that the crushed cerium carbonate particle powder was fired at 180 ° C. for 24 hours.
  • Example 3 101 g of cerium carbonate particle powder having a plate-like particle shape was dissolved in 83 mL concentrated hydrochloric acid (12 mol / L) and then diluted with pure water to 1 mol / L. Then, 1 mol / L sodium hydroxide was added dropwise to the solution at a rate of 20 mL / min to neutralize the solution, and the mixture was decanted and filtered with filter paper to recover the filtered material. The filtrate was then dried at 60 ° C. for 24 hours to give cerium oxide particles. The mode pore diameter of the obtained cerium oxide particles was 729 nm. The obtained cerium oxide particles were treated in the same manner as in Example 1 to obtain an adsorbent (sample).
  • Example 1 cerium oxide particles and an adsorbent (sample) were obtained in the same manner as in Example 1 except that the pulverized cerium carbonate particle powder was fired at 280 ° C. for 12 hours.
  • the gradient of the fluorine ion concentration (mg / L) after the lapse of the breakthrough time that is, after the fluorine ion concentration (mg / L) exceeds 1 mg / L and reaches 10 mg / L, is determined. It is shown as the adsorption rate (mg / L / hr).
  • the above-mentioned slope of the fluorine ion concentration is an index of the ease of adsorption of the adsorbent, and it can be said that the larger the slope, the better the adsorption reaction of the adsorbent. The larger the inclination, the better the adsorption efficiency, so the period until the next replacement can be lengthened.
  • the most frequent pore diameter of the anionic adsorbent made of a molded product containing cerium oxide is less than 80 nm and the total pore specific surface area. It was found that an adsorbent having a surface area of 10 m 2 / g or more can effectively adsorb anions in wastewater. Since this adsorbent has a large number of small-diameter pores and a high specific surface area of all pores, it has many anion adsorption points and has an anion adsorption performance. Can be inferred to be high.

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  • Chemical & Material Sciences (AREA)
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PCT/JP2020/034898 2019-10-03 2020-09-15 吸着材 Ceased WO2021065481A1 (ja)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120031827A1 (en) * 2010-08-06 2012-02-09 Molycorp Minerals, Llc Agglomeration of high surface area rare earths
JP2017512631A (ja) * 2014-03-07 2017-05-25 セキュア ナチュラル リソーシズ エルエルシーＳｅｃｕｒｅ Ｎａｔｕｒａｌ Ｒｅｓｏｕｒｃｅｓ Ｌｌｃ 極めて優れたヒ素除去特性を備える酸化セリウム（ｉｖ）
WO2017199919A1 (ja) * 2016-05-16 2017-11-23 日立化成株式会社 吸着剤、二酸化炭素の除去方法、二酸化炭素除去器、及び、空調装置
JP2019118877A (ja) * 2018-01-04 2019-07-22 旭化成株式会社 多孔性成形体

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20120031827A1 (en) * 2010-08-06 2012-02-09 Molycorp Minerals, Llc Agglomeration of high surface area rare earths
JP2017512631A (ja) * 2014-03-07 2017-05-25 セキュア ナチュラル リソーシズ エルエルシーＳｅｃｕｒｅ Ｎａｔｕｒａｌ Ｒｅｓｏｕｒｃｅｓ Ｌｌｃ 極めて優れたヒ素除去特性を備える酸化セリウム（ｉｖ）
WO2017199919A1 (ja) * 2016-05-16 2017-11-23 日立化成株式会社 吸着剤、二酸化炭素の除去方法、二酸化炭素除去器、及び、空調装置
JP2019118877A (ja) * 2018-01-04 2019-07-22 旭化成株式会社 多孔性成形体

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