CN104994934A - Water absorbent and method for producing same - Google Patents

Water absorbent and method for producing same Download PDF

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Publication number
CN104994934A
CN104994934A CN201480004347.1A CN201480004347A CN104994934A CN 104994934 A CN104994934 A CN 104994934A CN 201480004347 A CN201480004347 A CN 201480004347A CN 104994934 A CN104994934 A CN 104994934A
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polar solvent
aprotic polar
moisture adsorbent
calcium oxide
moisture
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CN104994934B (en
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渡边高行
本明纮
三岛拓也
佐野聡
植木明
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Ube Chemical Industries Co Ltd
Ube Material Industries Ltd
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Ube Chemical Industries Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/28—Selection of materials for use as drying agents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • 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
    • B01J20/041—Oxides or hydroxides
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/02—Oxides or hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/404—Alkaline earth metal or magnesium compounds of calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B01D2253/1124—Metal oxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/20—Organic adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/306—Surface area, e.g. BET-specific surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Drying Of Gases (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

Provided are: a water absorbent which can be produced at a low cost, is highly dispersible and hydrophobic, and does not exhibit a decline in moisture-absorption speed; and a method for producing the same. This water absorbent is characterized by having, as the principal component thereof, calcium oxide particles having an aprotic polar solvent layer on the surface thereof. The method for producing the water absorbent is characterized by crushing calcium oxide in the presence of an aprotic polar solvent. It is preferable for the aprotic polar solvent to be N-methylpyrrolidone.

Description

Moisture adsorbent and manufacture method thereof
Technical field
The invention relates to a kind of moisture adsorbent and manufacture method thereof.More specifically, be especially with surface, there is the moisture adsorbent and manufacture method thereof that the calcium oxide particle of aprotic polar solvent layer is principal component with comparatively useful as organic el element about a kind of.
Background technology
Luminous organic material for organic el element has the deterioration because of moisture, the problem of lifetime, since previously, configured hygroscopic materials (water absorbing agent) in order to the moisture residued in when being absorbed in the manufacture of EL assembly in assembly or the moisture infiltrated from outside.
Water absorbing agent is owing to requiring to seal rear rapid adsorption moisture, so use has the calcium oxide of barium monoxide or strontium oxide strontia or quickening water adsorption speed.Further, the calcium oxide accelerating water adsorption speed such as patent document 1 disclose, obtain by burning till calcium hydroxide under reduced pressure.
Patent document 1: Japan Patent No. 4387870 publication.
Summary of the invention
But, to burn till and the calcium oxide that obtain has following problem through decompression as described in Patent Document 1: (1) manufactures must vacuum firing stove, so be high cost; (2) owing to being strong basicity, so use in being filled in the high-molecular organic materials such as resin situation time, have the problem cutting off high molecular key, only can be used for a part of resins such as fluororesin; (3) calcium oxide is hydrophily, so be not easily filled to the high-molecular organic materials such as hydrophobic resin.
Previously, as the method for the problem of solution these (2) and (3), there will be a known the method utilizing the hydrophobic surface treating agent coats particle surfaces such as aliphatic acid, but about the purposes of organic el element etc., carry out hydrophobicity if having to be coated with, the low reduction of rate of moisture absorption, the problem that the performance as hygroscopic agent originally reduces.
The present invention forms in view of the above problems, its object is to provide a kind of and can be manufactured at low cost with, has higher dispersiveness and hydrophobicity and the moisture adsorbent that do not reduce of rate of moisture absorption and manufacture method thereof.
The present inventor etc. endeavour to study to reach the above object, found that: the calcium oxide particle that surface exists the thinner liquid layer of aprotic polar solvent can suppress aggegation and keep higher by dispersiveness, there is hydrophobicity and higher rate of moisture absorption and there is the drier institute preferably function as being filled in macromolecular material, thus completing the present invention.That is, the invention relates to a kind of moisture adsorbent, it is characterized in that: it has the calcium oxide particle of aprotic polar solvent layer for principal component with surface.
Again, the discoveries such as the present inventor: pulverize calcium oxide under existing in aprotic polar solvent, can obtain micronize and improve activity and have the calcium oxide particle of hydrophobicity, hygroscopicity excellence, thus completing the present invention.That is, the invention relates to a kind of manufacture method of moisture adsorbent, it is characterized in that: under aprotic polar solvent exists, dry type pulverizing is carried out to calcium oxide.Again, the invention relates to a kind of manufacture method of moisture adsorbent, it is characterized in that: after case of wet attrition is carried out under aprotic polar solvent exists to calcium oxide, carry out Separation of Solid and Liquid and/or drying.
As previously discussed, according to the present invention, can provide a kind of and can be manufactured at low cost with, there is higher dispersiveness and hydrophobicity and the moisture adsorbent that do not reduce of rate of moisture absorption and manufacture method thereof.
Detailed description of the invention
The feature of moisture adsorbent of the present invention is: it has the calcium oxide particle of aprotic polar solvent layer for principal component with surface.Aprotic polar solvent sex layer exists in the surface of calcium oxide particles, such as list: acetone, acetonitrile, N, N - dimethyl formamide (DMF), dimethyl sulfoxide (DMSO), N, N - dimethyl acetamide, tetrahydrofuran, two mouth e alkanes, six methyl phosphate three amine (hexamethylphosphotriamide), ethylene glycol dimethyl ether, acrylic nitrile, methyl ethyl ketone, diethylene glycol dimethyl ether, ethylene glycol dimethyl ether, etc. The layer, N - methyl pyrrole especially in optimizing the use of N - methyl pyrrole layer in the.In moisture adsorbent of the present invention, the thickness of aprotic polar solvent layer can define as following mathematical expression 1, is preferably 0.2 ~ 5nm.
[mathematical expression 1]
Again, the BET specific surface area of moisture adsorbent of the present invention is preferably 1 ~ 100m 2/ g, is more preferably 5 ~ 100m 2/ g, and then be preferably 10 ~ 60m 2/ g.If BET specific surface area is too small, then water adsorption slows, so not good, if excessive, then water adsorption excessive velocities, become be difficult to operation and undesirable.Again, average grain diameter is preferably 0.05 ~ 10 μm, is more preferably 0.2 ~ 5 μm, and then is preferably 0.5 ~ 3 μm.If average grain diameter is too small, then adsorption rate is too fast, becomes and is difficult to operation and undesirable, if excessive, and degraded appearance and undesirable in time being coated with or being used as filler.
As the mechanism of the function of performance moisture adsorbent of the present invention, think that the polarity of the aprotic polar solvent layer being present in calcium oxide surface gives hygroscopicity and the compatibility with calcium oxide, aprotic gives the intermiscibility (dissolving resin) to resin.Think that aprotic polar solvent layer is different from the situation being such as coated with alkoxide layer on calcium oxide surface, reactions such as " alkoxide hydrolysis and resolve into water and alcohol; generate alkoxide because of the reaction of alcohol and calcium oxide " is not caused, so the hygroscopicity higher than the coating being attended by above-mentioned reaction can be played due to it.In moisture adsorbent of the present invention, as hygroscopic evaluation, such as can evaluate according to the weight increase of the moisture adsorbent of (temperature 24 DEG C, relative humidity 55%) after 120 minutes, above-mentioned weight increase is preferably more than 10%, and then is preferably 10 ~ 30%.
Moisture adsorbent of the present invention, by after carrying out dry type pulverizing or case of wet attrition to calcium oxide under aprotic polar solvent exists, is optionally carried out drying process, is adjusted the thickness of aprotic polar solvent layer and manufacture.In time carrying out the situation of case of wet attrition, after also carrying out Separation of Solid and Liquid by filtration etc., carry out drying process.
In the manufacture method of moisture adsorbent of the present invention, as the BET specific surface area of the calcium oxide of raw material, there is no particular restriction, is preferably 0.1 ~ 60m 2/ g, is more preferably 0.5 ~ 30m 2/ g.Again, there is no particular restriction for the average grain diameter of calcium oxide, is preferably 0.1 μm ~ 5mm.
In manufacture method of the present invention, as used aprotic polar solvent, can enumerate and the identical person of above-mentioned aprotic polar solvent layer, these can be used alone or mix two or more use.When the situation that dry type is pulverized, the use amount of aprotic polar solvent, relative to calcium oxide, is preferably 0.1 ~ 51 quality %, is more preferably 1 ~ 20 quality %, and then is preferably 1 ~ 15 quality %.If use aprotic polar solvent to pulverize, then solvent plays the effect as grinding aid, can be crushed to fine and that activity is higher particulate under the state guaranteeing higher dispersiveness.When the situation of case of wet attrition, the use amount of aprotic polar solvent, relative to calcium oxide, is preferably 52 ~ 10000 quality %, is more preferably 500 ~ 5000 quality %, is especially preferably 1000 ~ 2000 quality %.Again, the boiling point of aprotic polar solvent is preferably more than 100 DEG C, is more preferably more than 150 DEG C.If boiling point does not reach 100 DEG C, then because aprotic polar solvent layer becomes easy volatilization, so not good.
In the present invention, the method for pulverizing is not particularly limited, and can use medium grinder, rotating ball mill, vibrator, planetary ball mill, the reducing mechanism such as (rocking mill), coating vibrating machine, jet mill that waves grinding machine.Be preferably medium grinder among reducing mechanism, wave grinding machine etc. use metal or resin, pottery medium as the reducing mechanism of medium.The material of medium is with regard to viewpoint of reduced contamination, and more satisfactory is nylon or wear away less zirconia system.Moreover the large I of medium is suitably selected according to by the particle diameter of crushed material.Again, pulverizing is preferably carried out in non-reactive gas ambient.As non-active gas, though also can helium or argon gas etc. be enumerated, with regard to economic viewpoint, especially preferably carry out in nitrogen environment.Moreover pulverization process can be carried out by one-phase, also replaceable medium footpath or reducing mechanism and pulverize with the multistage.
Again, 90% particle diameter (D of the size distribution of moisture adsorbent of the present invention 90) and 10% particle diameter (D 10) ratio D 90/ D 10be preferably in the scope of 1.5 ~ 40, be more preferably and make size distribution steepen (sharp) be in the scope of 1.5 ~ 5.0.
When this situation, in jet mill especially jet mill due to the powder of fine and precipitous size distribution can be obtained, so better.If size distribution is precipitous, then due to the rate of moisture absorption stabilisation of calcium oxide, so better.And then, jet mill owing to being sized particles in air-flow, so the aprotic polar solvent of particle surface partly can be removed.Therefore, the advantage that can simplify or omit drying process is had.Moreover, as the pulverization conditions utilizing jet mill, such as, under raw material supplying speed 5.0kg/h, by pulverizing pressure is set to 0.3 ~ 1.5MPa, is more preferably and is set to 0.3 ~ 1.0MPa, can as mentioned above by D 90/ D 10steepen is in the scope of 1.5 ~ 5.0.
Again, dry process is carried out preferably by heat drying, also can carry out drying under reduced pressure, as drying device, can enumerate laminated board type (shelf type) drying machine, spin-drier, vibrating drier, vacuum drier etc.The drying with the calcium oxide particle of aprotic polar solvent layer preferably simultaneously imports the non-active gas such as nitrogen or argon gas one side and carries out, to avoid making aprotic polar solvent layer decompose because of the reaction with the steam in environment or carbon dioxide or producing calcium hydroxide or calcium carbonate in drying machine.The temperature of heat drying process is below the boiling point of aprotic polar solvent layer, such as, when the situation of N-methylpyrrole pyridine ketone, be preferably 80 ~ 180 DEG C, be more preferably 120 ~ 170 DEG C.Moreover, in time carrying out by case of wet attrition the situation manufactured, more satisfactory for carrying out drying process after the equipment for separating liquid from solid by filtration or centrifugation etc. removes unnecessary solvent.Removing unnecessary solvent by suitably adjusting drying condition, the thickness of aprotic polar solvent layer can be adjusted to specific value.
According to the present invention, can be manufactured at low cost with and there is higher dispersiveness and hydrophobicity and the moisture adsorbent that rate of moisture absorption does not reduce compared with common calcium oxide.And then moisture adsorbent of the present invention has volume density (bulk density) and is filled in resin more greatly and easily, oil absorption is less and can the highly-filled effect excellent in resin etc.Moreover oil absorption evaluates powder to the index of the fillibility of resin, and the method can be used for the evaluation (magazine " industrial materials " vol.39, No.1, p116-117 (1991)) of fillibility.The oil absorption of moisture adsorbent of the present invention is preferably below 45ml/100g.
Moisture adsorbent of the present invention can directly use or be configured as arbitrary shape and use.Again, can be made into the coating being filled in suitable solvent or macromolecular material, the adhesive tape being filled in macromolecular material or film etc. and use.Therefore, thermal insulation layer drier, the water adsorption layer of Obstruct membrane, liner use (preventing the deterioration of chemicals, pharmaceuticals, food) of closed container, the inner face coating use, O shape ring use (maintenance high vacuum) etc. of vacuum line that organic EL, liquid crystal etc. avoid the electronic equipment drier, refrigerator, double glazing etc. keeping away moisture can be also preferably used for.
Wherein, moisture adsorbent of the present invention especially can preferably be used as organic el element use.Such as, organic el element moisture adsorbent dispersibles to form in synthetic resin and forms sheet, graininess, tabular, membranaceous and be used.These moldings can be used as the drier of the e-machines such as organic el display and advantageously use.Synthetic resin can use vistanex, polyacrylic resin, polyacrylonitrile resin, polyamide, mylar, epoxy resin, polycarbonate resin and fluororesin.Again, moisture adsorbent of the present invention also can be contained in the bag of the poisture-penetrability that common hygroscopic agent uses or container and to use.Moisture adsorbent of the present invention can be used alone, and also can use with other hygroscopic materials (such as silica gel or molecular sieve).
Embodiment
Below, be specifically described the present invention is based on embodiment, but these and non-limiting object person of the present invention.First, the assay method of the physical property of the lime powder of acquisition is shown in following.
[hygroscopicity evaluation: the weight increase after 120 minutes]
Measure the weight of dry measuring cup in advance, be set to [A (g)].The powder becoming determination object is about 0.6g to be loaded in measuring cup, and weigh is exactly set to [B (g)].Open the lid of the measuring cup that powder is housed, putting into remaining 24 DEG C, the constant temperature and humidity cabinet of relative humidity 55%, measuring the weight after 120 minutes, being set to [C (g)], calculating weight increase by following formula (1).
[mathematical expression 2]
Weight increase (%)={ C (g)-B (g) }/B (g)-A (g)) × 100 (1)
[assay method of oil absorption]
According to JIS K 5101-13-2:2004 pigment test method-13: oil absorption-Section 2: boil flaxseed oil process and measure.The powdered sample of specified quantitative is dripped and boils linseed oil, according to boil that sample that linseed oil mixes becomes can the dripping quantity of terminal of state of twist up, obtain oil absorption (mL/100g).
[assay method of size distribution]
Use ethanol as the dispersion solvent of sample, utilize ultrasonic homogenizer (MODEL US-150T, this smart machine-processed Zuo Suo limited company of order manufactures) to carry out 3 minutes dispersion treatment.Laser diffraction method particle size distribution device (MICROTRAC HRA9320-X100 is used to the sample of dispersion, Ji Zhuan limited company manufacture) or dynamic light scattering method particle size distribution device (manufacture of Nanotrac UPA-EX150, Ji Zhuan limited company) carry out size distribution (D 10, D 50, D 90) mensuration.
[assay method of BET specific surface area]
The mensuration of BET specific surface area uses Monosorb (Quantachrome manufacture) to be measured by BET single-point method.
[the dispersed evaluation method to organic solvent]
The dispersiveness evaluation of sample to organic solvent uses n-hexane to carry out.Get n-hexane 5ml in vial, add sample and be about 0.1g, vibrate after one minute and leave standstill, observe the situation of the solution after 30 seconds.If be scattered in hexane also muddy, then be evaluated as the favorable dispersibility (zero) of sample to organic solvent, if aggegation in hexane, hexane maintains transparent state and sample Shen Dian, be then evaluated as the dispersiveness of sample to organic solvent poor (×).
[assay method of volume density]
In the glove box being filled with nitrogen, sample is filled to volume 4.4cm gently 3quartz container (bottom surface 10mm × 10mm, height 44mm), fully fill.The surface of floating powder, weighs sample weight exactly, is set to [D (g)], calculates volume density by following formula (2).
[mathematical expression 3]
Volume density (g/cm 3)=D (g)/4.4 (cm 3) (2)
[computational methods of coating layer thickness]
According to the weight reduced from 20 DEG C to 250 DEG C recorded by thermobalance (TG), calculate the quality of aprotic polar solvent (being N-methylpyrrole pyridine ketone in embodiment 1), divided by the proportion (being 1.028 when the situation of N-methylpyrrole pyridine ketone) of solvent, calculate the solvent volume relative to every 1g calcium oxide.The surface area of every 1g calcium oxide of it being tried to achieve divided by being measured by BET specific surface area, calculates the thickness of coating and aprotic polar solvent thus.
[assay method of FT-IR]
The mensuration of FT-IR divides luminometer (FT/IR-6100, Japanese light splitting limited company manufactures) assembling individual reflection determinator (ATR PRO470-H) to measure in fourier-transform infrared.The scope of the wave number measured is 4000 ~ 400cm -1.
[embodiment 1]
In 100mL closed container (polypropylene system), add zirconia pearl (manufacture of the Nikkato limited company) 120g of diameter phi 4.0mm, burn till granular product (the BET specific surface area 16.5m of high-specific surface area calcium oxide of the granulation product of calcium hydroxide micropowder with 600 DEG C 2/ g, granularity 2 ~ 3mm) 6g and N-methylpyrrole pyridine ketone 0.45g sealing.Above operation carries out in the glove box being filled with nitrogen, and this closed container is filled by nitrogen.Grinding machine (manufacture of SEIWA GIKEN limited company) is waved in this closed container taken out from glove box utilization and carries out 4 hours pulverization process with 700rpm.After process, in the glove box being filled with nitrogen, use the screening of mesh 1mm from zirconia pearl and lime powder.Utilized by the lime powder be separated, reclaim laminated board type drying machine to carry out dry process in 18 hours with 150 DEG C in nitrogen environment, obtain the lime powder of the embodiment 1 being covered particle surface by aprotic polar solvent layer.The average grain diameter of the lime powder obtained is 1.24 μm, volume density is 0.77g/cm 3.Other physical property are shown in table 1.
[comparative example 1]
Use high-purity mangesium oxide calcium powder (ultra-high purity calcium oxide (CSQ), BET specific surface area 2.3m 2/ g, average grain diameter 16.5 μm, Ube Material Industries limited company manufactures).The average grain diameter of this lime powder is 16.5 μm, volume density is 0.69g/cm 3.Other physical property are shown in table 1.
[comparative example 2]
Use the calcium oxide (how rice powder diameter < 160nm (BET)) that Sigma-Aldrich manufactures.The average grain diameter of this lime powder is 0.87 μm, volume density is 0.21g/cm 3.Other physical property are shown in table 1.
[comparative example 3]
Diethyl ether 40mL is utilized to dissolve stearic acid 0.065g.In this solution, add calcium oxide (how rice powder diameter < 160nm (BET)) 1.3g that Sigma-Aldrich manufactures and mix 10 minutes.Mixed solution is removed solvent in 30 DEG C of vacuum drying 12 hours.In the glove box being filled with nitrogen, use agate mortar to carry out crushing process to the xeraphium reclaimed, obtain the lime powder using aliphatic acid to carry out surface-treated comparative example 3.The average grain diameter of the lime powder obtained is 0.86 μm, volume density is 0.79g/cm 3.Other physical property are shown in table 1.
[comparative example 4]
Zirconia pearl (manufacture of Nikkato limited company) 120g, high-purity mangesium oxide calcium powder (ultra-high purity calcium oxide (CSQ), the BET specific surface area 2.3m of diameter phi 4.0mm is added in 100mL closed container (polypropylene system) 2/ g, average grain diameter 16.5 μm, Ube Material Industries limited company manufactures) 6g and ethanol 0.45g sealing.More than operation carries out in the glove box being filled with nitrogen, and this closed container is filled by nitrogen.Grinding machine (manufacture of SEIWA GIKEN limited company) is waved in this closed container taken out from glove box utilization and carries out 4 hours pulverization process with 700rpm.After process, in the glove box being filled with nitrogen, the sieve of 500 μm, mesh is used to be separated with lime powder by zirconia pearl.Utilize laminated board type drying machine in nitrogen environment, to carry out 18 hour dry process with 150 DEG C to the lime powder being separated, reclaiming, obtain the lime powder of the comparative example 4 being covered particle surface by alkoxide.Confirm that the surface of obtained lime powder exists alkoxide layer by FT-IR.The average grain diameter of the lime powder obtained is 0.83 μm, volume density is 0.86g/cm 3.Other physical property are shown in table 1.
[embodiment 2]
Calcium hydroxide micropowder (BET specific surface area 13m will be burnt till with 600 DEG C 2/ g, average grain diameter 5.6 μm) and lime powder (the BET specific surface area 15m of acquisition 2/ g, average grain diameter 5.1 μm) 3000g and N-methylpyrrole pyridine ketone 105g uses the mixer of internal volume 33L (the New-Gra Machine:SEG-350 type that SEISHINENTERPRISE limited company manufactures) to mix equably under nitrogen environment.Utilize jet mill (the STJ-200 type that SEISHIN ENTERPRISE limited company manufactures) to carry out pulverization process under the condition of raw material supplying speed 5.0kg/h, pulverizing pressure 0.7MPa to the lime powder reclaimed from mixer, obtain the lime powder of the embodiment 2 being covered particle surface by aprotic polar solvent layer.During pulverization process, compressed fluid uses nitrogen, and then, surround reducing mechanism entirety with cell (booth), little indoor are set to nitrogen environment, avoid powder to contact with air thus as far as possible.The physical property of the lime powder obtained is shown in table 1.
[embodiment 3]
The amount of N-methylpyrrole pyridine ketone is set to 210g, in addition, manufactures with the method identical with embodiment 2, obtain the lime powder of the embodiment 3 being covered particle surface by aprotic polar solvent layer.The physical property of the lime powder obtained is shown in table 1.
[table 1]

Claims (7)

1. a moisture adsorbent, it has the calcium oxide particle of aprotic polar solvent layer for principal component with surface.
2. moisture adsorbent according to claim 1, wherein, this aprotic polar solvent is N-methylpyrrole pyridine ketone.
3. an organic el element moisture adsorbent, it uses moisture adsorbent according to claim 1 and 2.
4. the manufacture method of a moisture adsorbent: under aprotic polar solvent exists, dry type pulverizing is carried out to calcium oxide.
5. the manufacture method of a moisture adsorbent: after case of wet attrition is carried out under aprotic polar solvent exists to calcium oxide, carry out Separation of Solid and Liquid and/or drying.
6. the manufacture method of the moisture adsorbent according to claim 4 or 5, wherein, this aprotic polar solvent is N-methylpyrrole pyridine ketone.
7. the manufacture method of the moisture adsorbent according to any one of claim 4 to 6, wherein, this moisture adsorbent is that organic el element is used.
CN201480004347.1A 2013-01-10 2014-01-08 Moisture adsorbent and its manufacture method Active CN104994934B (en)

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JP2013-002920 2013-01-10
JP2013002920 2013-01-10
PCT/JP2014/050136 WO2014109330A1 (en) 2013-01-10 2014-01-08 Water absorbent and method for producing same

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CN104994934B CN104994934B (en) 2017-08-22

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