CN104994934B - Moisture adsorbent and its manufacture method - Google Patents
Moisture adsorbent and its manufacture method Download PDFInfo
- Publication number
- CN104994934B CN104994934B CN201480004347.1A CN201480004347A CN104994934B CN 104994934 B CN104994934 B CN 104994934B CN 201480004347 A CN201480004347 A CN 201480004347A CN 104994934 B CN104994934 B CN 104994934B
- Authority
- CN
- China
- Prior art keywords
- moisture adsorbent
- polar solvent
- manufacture method
- aprotic polar
- calcium oxide
- Prior art date
- Legal status (The legal status 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 status listed.)
- Active
Links
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (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
The present invention provides a kind of moisture adsorbent and its manufacture method that can be manufactured at low cost with, do not reduced with higher dispersiveness and hydrophobicity and rate of moisture absorption.The moisture adsorbent of the present invention is characterised by：It has the calcium oxide particle of aprotic polar solvent layer as principal component using surface.Also, the manufacture method of the moisture adsorbent of the present invention is characterised by：Calcium oxide is crushed in the presence of aprotic polar solvent.Above-mentioned aprotic polar solvent is preferably 1-METHYLPYRROLIDONE.
Description
Technical field
The present invention is on a kind of moisture adsorbent and its manufacture method.More specifically, it is especially to make on one kind
There is the calcium oxide particle of aprotic polar solvent layer as the water of principal component using surface with more useful for organic el element
Divide adsorbent and its manufacture method.
Background technology
Luminous organic material for organic el element has to be deteriorated because of moisture, the problem of lifetime, since previously,
Hygroscopic materials are configured for the moisture that residues in component when being absorbed in the manufacture of EL components or from the moisture that outside is penetrated into
(water absorbing agent).
Water absorbing agent is due to requiring rapid adsorption moisture after sealing, so using having barium monoxide or strontium oxide strontia or accelerate water
Divide the calcium oxide of adsorption rate.Also, accelerate the calcium oxide of water adsorption speed for example as disclosed in patent document 1, can pass through
Obtained in burning till calcium hydroxide under reduced pressure.
Patent document 1：No. 4387870 publications of Japanese Patent No..
The content of the invention
However, as described in Patent Document 1 through decompression burn till obtained by calcium oxide there is following problem：(1) manufacture must
Vacuum firing stove is needed, so be high cost；(2) due to for strong basicity, so in being filled in the high-molecular organic materials such as resin and
During the situation used, the problem of having cut-out high molecular key can only be used to a part of resin such as fluororesin；(3) calcium oxide is parent
It is aqueous, so filling is difficult to high-molecular organic materials such as hydrophobic resins.
Previously, as method the problem of solving these (2) and (3), it is known to utilize the hydrophobic surfaces such as aliphatic acid
The method on inorganic agent coated particle surface, but on the purposes of organic el element etc., there is the moisture absorption speed if hydrophobicity coating is carried out
Spend sinking low, the problem of reduction as the performance of hygroscopic agent of script.
The present invention is formed in view of the above problems, and its object is to provide one kind to can be manufactured at low cost with, with higher
Dispersiveness and hydrophobicity and the rate of moisture absorption moisture adsorbent and its manufacture method that do not reduce.
The present inventor etc. endeavour to be studied to reach the above object, as a result find：There is aprotic in surface
The calcium oxide particle of the relatively thin liquid layer of polar solvent can suppress aggegation and dispersiveness is kept as it is higher, with hydrophobicity with compared with
High rate of moisture absorption and with as the drier for being filled in high polymer material preferably function, so as to complete the present invention.That is,
The present invention is on a kind of moisture adsorbent, it is characterised in that：It has the calcium oxide of aprotic polar solvent layer with surface
Particle is principal component.
Also, the present inventor etc. has found：By crushing calcium oxide in the presence of aprotic polar solvent, micronized can be obtained
And improve activity and there is the excellent calcium oxide particle of hydrophobicity, hygroscopicity, so as to complete the present invention.That is, the present invention be on
A kind of manufacture method of moisture adsorbent, it is characterised in that：Dry type is carried out in the presence of aprotic polar solvent to calcium oxide
Crush.Also, the present invention is on a kind of manufacture method of moisture adsorbent, it is characterised in that：To calcium oxide in aprotic pole
Property solvent in the presence of carry out after case of wet attrition, carry out separation of solid and liquid and/or drying.
As previously discussed, according to the present invention, it is possible to provide a kind of to can be manufactured at low cost with, with higher dispersed and hydrophobic
Moisture adsorbent and its manufacture method that property and rate of moisture absorption are not reduced.
Embodiment
The moisture adsorbent of the present invention is characterised by：It has the calcium oxide grain of aprotic polar solvent layer with surface
Son is principal component.Aprotic polar solvent layer is present in the calcium oxide particle surface, for example, can enumerate：Acetone, acetonitrile, N,
Dinethylformamide (DMF), dimethyl sulfoxide (DMSO) (DMSO), DMAC N,N' dimethyl acetamide, tetrahydrofuran, Er Kou e alkane, six
Methyl acid phosphate triamine (hexamethylphosphotriamide), glycol dimethyl ether, propionitrile, methyl ethyl ketone, diethylene glycol
The layer of dimethyl ether, TRIGLYME, 1-METHYLPYRROLIDONE etc., especially preferably uses 1-METHYLPYRROLIDONE
Layer.In the moisture adsorbent of the present invention, the thickness of aprotic polar solvent layer can be determined such as following mathematical expressions 1
Justice, preferably 0.2~5nm.
[mathematical expression 1]
Also, the BET specific surface area of the moisture adsorbent of the present invention is preferably 1~100m2/ g, more preferably 5~100m2/ g,
And then preferably 10~60m2/g.If BET specific surface area is too small, water adsorption slows, so it is not good, if excessive,
Water adsorption excessive velocities, it becomes difficult to operation and it is undesirable.Also, average grain diameter is preferably 0.05~10 μm, more preferably 0.2
~5 μm, and then preferably 0.5~3 μm.If average grain diameter is too small, adsorption rate is too fast, it becomes difficult to operation and it is undesirable,
If if excessive in coating or during as filler degraded appearance and it is undesirable.
It is used as the mechanism of the function of the moisture adsorbent of the performance present invention, it is believed that be present in the aprotic on calcium oxide surface
The polarity of polar solvent, layer assigns hygroscopicity and the compatibility with calcium oxide, and aprotic assigns the intermiscibility (dissolving to resin
Resin).Think that aprotic polar solvent layer is different from the situation for being for example coated with alkoxide layer on calcium oxide surface, due to it
Do not cause reactions such as " alkoxide are hydrolyzed and resolves into water and alcohol, and alkoxide is generated because of the reaction of alcohol and calcium oxide ",
So it can play than being coated with high hygroscopicity with above-mentioned reaction.In the moisture adsorbent of the present invention, hygroscopicity is used as
Evaluation, can for example be carried out according to the weight increase of the moisture adsorbent of (24 DEG C of temperature, relative humidity 55%) after 120 minutes
Evaluate, above-mentioned weight increase is preferably more than 10%, and then preferably 10~30%.
The moisture adsorbent of the present invention can be by carrying out dry grinding to calcium oxide in the presence of aprotic polar solvent
Or after case of wet attrition, processing, the thickness of adjustment aprotic polar solvent layer is optionally dried and manufactures.In progress wet type
During the situation of crushing, drying process is carried out after also can carrying out separation of solid and liquid by filtering etc..
In the manufacture method of the moisture adsorbent of the present invention, the BET specific surface area of the calcium oxide as raw material has no spy
Do not limit, preferably 0.1~60m2/ g, more preferably 0.5~30m2/g.Also, there is no particular restriction for the average grain diameter of calcium oxide,
Preferably 0.1 μm~5mm.
In the present invention manufacture method in, as used aprotic polar solvent, can enumerate with it is above-mentioned non-proton
The property identical person of polar solvent, layer, these can be used alone or mix two or more use.It is non-proton when the situation of dry grinding
The usage amount of property polar solvent is relative to calcium oxide, preferably 0.1~51 mass %, more preferably 1~20 mass %, Jin Eryou
Elect 1~15 mass % as.If being crushed using aprotic polar solvent, solvent plays the effect as grinding aid,
Fine and active higher particulate can be crushed in the state of higher dispersiveness is ensured.When the situation of case of wet attrition,
The usage amount of aprotic polar solvent is relative to calcium oxide, preferably 52~10000 mass %, more preferably 500~5000
Quality %, preferably especially 1000~2000 mass %.Also, the boiling point of aprotic polar solvent is preferably more than 100 DEG C, it is more excellent
Elect more than 150 DEG C as.If boiling point is not up to 100 DEG C, because aprotic polar solvent layer becomes readily volatilized, so it is not good.
In the present invention, the method for crushing is not particularly limited, and medium grinder, rotating ball mill, vibrating ball can be used
Grinding machine, planetary ball mill, wave the reducing mechanisms such as grinding machine (rocking mill), coating vibrating machine, jet mill.Crush
Be preferably medium grinder among device, wave grinding machine etc. and use metal or resin, the medium of ceramics as medium crushing dress
Put.The material of medium is for viewpoint of reduced contamination, and more satisfactory is nylon system or the less zirconium oxide system of abrasion.Furthermore, it is situated between
The big I of matter is suitably selected according to the particle diameter of pulverized thing.Also, it is preferably to be carried out in non-reactive gas ambient to crush.As
Non-active gas, though can also enumerate helium or argon gas etc., for economic viewpoint, outstanding is preferably to enter in nitrogen environment
OK.Furthermore, pulverization process can be carried out with a stage, also replaceable medium footpath or reducing mechanism and crushed with the multistage.
Also, 90% particle diameter (D of the size distribution of the moisture adsorbent of the present invention90) and 10% particle diameter (D10) ratio D90/
D10In the range of preferably 1.5~40, in the range of more preferably making size distribution change precipitous (sharp) into 1.5~5.0.
When the situation, especially jet mill is due to that can obtain fine and precipitous size distribution in jet mill
Powder, so preferably.If size distribution is precipitous, because the rate of moisture absorption of calcium oxide is stabilized, so preferably.And then, spray
Grinding machine is penetrated due to being the sized particles in air-flow, so can partly remove the aprotic polar solvent of particle surface.Therefore,
Have the advantages that to simplify or omit drying process.Furthermore, as the pulverization conditions using jet mill, for example, supply speed in raw material
Spend under 5.0kg/h, be set to 0.3~1.5MPa by the way that pressure will be crushed, be more preferably set to 0.3~1.0MPa, can be as described above
By D90/D10Become precipitous in the range of 1.5~5.0.
Also, drying process is carried out preferably by heat drying, it can be also dried under reduced pressure, can as drying device
Enumerate laminated board type (shelf type) drying machine, spin-drier, vibrating drier, vacuum drier etc..With non-matter
The drying of the calcium oxide particle of sub- property polar solvent, layer is preferably one side in the importing nonactive gas such as nitrogen or argon gas in drying machine
Body one side is carried out, to avoid making because of the reaction with vapor or carbon dioxide in environment aprotic polar solvent layer decomposition
Or produce calcium hydroxide or calcium carbonate.Below boiling point of the temperature of heat drying processing for aprotic polar solvent layer, example
It is preferably 80~180 DEG C such as when the situation of 1-METHYLPYRROLIDONE, more preferably 120~170 DEG C.Furthermore, in passing through wet type
When crushing the situation manufactured, more satisfactory is unnecessary molten in the equipment for separating liquid from solid removal by filtering or centrifuging etc.
Drying process is carried out after agent.Unnecessary solvent is removed by suitably adjusting drying condition, can be by aprotic polar solvent layer
Thickness be adjusted to specific value.
According to the present invention it is possible to which low cost manufacture is with higher dispersiveness and hydrophobicity and compared with common calcium oxide
The moisture adsorbent that rate of moisture absorption is not reduced.And then, moisture adsorbent of the invention have volume density (bulk density) compared with
Greatly and be easily filled in resin, oil absorption it is smaller and can the highly-filled effect excellent in resin etc..Furthermore, oil absorption is to evaluate
Powder to the index of the fillibility of resin, this method can be used for fillibility evaluation (magazine " industrial materials " vol.39, No.1,
P116-117 (1991)).The oil absorption of the moisture adsorbent of the present invention is preferably below 45ml/100g.
The moisture adsorbent of the present invention can be used directly or be configured to arbitrary shape and uses.It is filled in also, can be made into
Appropriate solvent or the coating of high polymer material, the adhesive tape or film for being filled in high polymer material etc. and use.Therefore,
Also it can be preferably used as the thermal insulation layer of electronic equipment drier, refrigerator, the double glazing of the deterrent moisture such as organic EL, liquid crystal etc.
With drier, the water adsorption layer of Obstruct membrane, closed container pad with (deterioration for preventing chemicals, pharmaceuticals, food), true
The inner face coating of empty pipe arrangement is used, O-ring is used (maintenance high vacuum) etc..
Wherein, moisture adsorbent of the invention is especially preferably used as organic el element use.For example, organic el element
Be dispersed among with moisture adsorbent in synthetic resin and be shaped as sheet, it is graininess, tabular, membranaceous and be used.These into
Shape thing can advantageously be used as the drier of the e-machines such as organic el display.Polyolefin tree can be used in synthetic resin
Fat, polyacrylic resin, polyacrylonitrile resin, polyamide, polyester resin, epoxy resin, polycarbonate resin and fluorine tree
Fat.Also, the moisture adsorbent of the present invention can also be contained in the bag or container of penetrability used in common hygroscopic agent and make
With.The moisture adsorbent of the present invention can be used alone, and can be also used in combination with other hygroscopic materials (such as silica gel or molecular sieve).
Embodiment
Hereinafter, the present invention is specifically illustrated based on embodiment, but these and non-limiting purpose of the present invention person.It is first
First, the assay method of the physical property of the lime powder of acquisition is shown in following.
[hygroscopicity evaluation：Weight increase after 120 minutes]
The weight for the measuring cup that measured in advance is dried, is set to [A (g)].Powder as measure object about 0.6g is loaded
Into measuring cup, weight is weighed exactly, is set to [B (g)].The lid of the measuring cup equipped with powder is opened, is put into remaining 24
DEG C, the constant temperature and humidity cabinet of relative humidity 55%, measurement 120 minutes after weight, be set to [C (g)], calculated by following formula (1)
Weight increase.
[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 methods-the 13：Oil absorption-Section 2：Boil flax
Benevolence oil process is measured.Linseed oil is boiled in powdered sample dropwise addition to specified quantitative, according to the examination with boiling linseed oil kneading
Sample turn into can twist up state terminal dripping quantity, obtain oil absorption (mL/100g).
[assay method of size distribution]
Using ethanol as the dispersion solvent of sample, ultrasonic homogenizer (MODEL US-150T, this smart mechanism of mesh are utilized
Zuo Suo limited companies manufacture) carry out 3 minutes decentralized processings.Laser diffraction method particle size distribution is used to scattered sample
Device (manufacture of MICROTRAC HRA9320-X100, Ji Zhuan limited companies) or dynamic light scattering method size distribution are surveyed
Determine device (manufacture of Nanotrac UPA-EX150, Ji Zhuan limited companies) and carry out size distribution (D10、D50、D90) survey
It is fixed.
[assay method of BET specific surface area]
The measure of BET specific surface area is to be determined using Monosorb (Quantachrome manufactures) by BET single-point methods.
[to the dispersed evaluation method of organic solvent]
Sample, which is evaluated the dispersiveness of organic solvent, to be carried out using n-hexane.N-hexane 5ml is taken into vial, is added
Sample about 0.1g, vibration is stood after one minute, the situation of the solution after observing 30 seconds.If being scattered in hexane and muddy, comment
Valency be sample to the favorable dispersibility (zero) of organic solvent, if the aggegation in hexane, hexane maintains transparent state and sample Shen
Form sediment, be then evaluated as dispersed poor (×) of the sample to organic solvent.
[assay method of volume density]
In in the glove box filled with nitrogen, sample is gently filled to volume 4.4cm3Quartz container (bottom surface 10mm ×
10mm, height 44mm), fully fill.The surface of floating powder, weighs sample weight exactly, [D (g)] is set to, by following
Formula (2) calculates volume density.
[mathematical expression 3]
Volume density (g/cm3)=D (g)/4.4 (cm3) (2)
[computational methods of coating layer thickness]
According to by thermobalance (TG) measure from 20 DEG C to the weight of 250 DEG C of reductions, calculate aprotic polar solvent
The quality of (in embodiment 1 be 1-METHYLPYRROLIDONE), divided by the proportion of solvent (is when the situation of 1-METHYLPYRROLIDONE
1.028) solvent volume relative to every 1g calcium oxide, is calculated.The every 1g tried to achieve by it divided by by BET specific surface area measure
The surface area of calcium oxide, thus calculates the coating i.e. thickness of aprotic polar solvent.
[FT-IR assay method]
FT-IR measure is that (FT/IR-6100, Japanese light splitting share is limited in fourier-transform infrared light splitting luminance meter
Company manufacture) assembling individual reflection determine device (ATR PRO470-H) be measured.The scope of the wave number of measure be 4000~
400cm- 1。
[embodiment 1]
The addition diameter in 100mL closed containers (polypropylene system)Zirconium oxide pearl (Nikkato shares
Co., Ltd manufactures) 120g, the granulation product for burning till with 600 DEG C calcium hydroxide micropowder high-specific surface area calcium oxide it is granular
Product (BET specific surface area 16.5m2/ g, 2~3mm of granularity) 6g and 1-METHYLPYRROLIDONE 0.45g and seal.Operation above
It is, in progress in the glove box filled with nitrogen, this closed container is filled by nitrogen.By the closed appearance of the sheet taken out from glove box
Device using wave grinding machine (manufacture of SEIWA GIKEN limited companies) with 700rpm carry out 4 hours pulverization process.After processing,
In in the glove box filled with nitrogen, mesh 1mm sieve separation zirconium oxide pearl and lime powder are used.Will separation, recovery
Lime powder using laminated board type drying machine in nitrogen environment with 150 DEG C progress drying process in 18 hours, obtain by non-matter
The lime powder of the embodiment 1 of sub- property polar solvent, layer covering particle surface.The average grain diameter of the lime powder obtained
It is 0.77g/cm for 1.24 μm, volume density3.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 2.3m2/ g, average grain diameter
16.5 μm, the manufacture of Ube Material Industries limited companies).The average grain diameter of this lime powder is 16.5 μ
M, volume density are 0.69g/cm3.Other physical property are shown in table 1.
[comparative example 2]
The calcium oxide (nm powder diameter ＜ 160nm (BET)) manufactured using Sigma-Aldrich.This lime powder
Average grain diameter be 0.87 μm, volume density be 0.21g/cm3.Other physical property are shown in table 1.
[comparative example 3]
Utilize diethyl ether 40mL dissolving stearic acid 0.065g.The oxidation of Sigma-Aldrich manufactures is added in the solution
Calcium (nm powder diameter ＜ 160nm (BET)) 1.3g is simultaneously mixed 10 minutes.By mixed solution in 30 DEG C be dried in vacuo 12 hours and
Remove solvent.In carrying out crushing processing to the xeraphium of recovery using agate mortar in the glove box filled with nitrogen, made
The lime powder for the comparative example 3 being surface-treated with aliphatic acid.The average grain diameter of the lime powder obtained is
0.86 μm, volume density be 0.79g/cm3.Other physical property are shown in table 1.
[comparative example 4]
The addition diameter in 100mL closed containers (polypropylene system)Zirconium oxide pearl (Nikkato shares
Co., Ltd manufacture) 120g, high-purity mangesium oxide calcium powder (ultra-high purity calcium oxide (CSQ), BET specific surface area 2.3m2/ g, puts down
Equal 16.5 μm of particle diameter, the manufacture of Ube Material Industries limited companies) 6g and ethanol 0.45g and seal.With
Upper operation is, in progress in the glove box filled with nitrogen, this closed container is filled by nitrogen.The sheet that will be taken out from glove box
Closed container using wave grinding machine (manufacture of SEIWA GIKEN limited companies) with 700rpm carry out 4 hours pulverization process.Place
After reason, zirconium oxide pearl is separated with lime powder in the sieve in the glove box filled with nitrogen using 500 μm of mesh.Utilize
Laminated board type drying machine carries out drying process in 18 hours in nitrogen environment to separation, the lime powder reclaimed with 150 DEG C, obtains
The lime powder of the comparative example 4 of particle surface is covered by alkoxide.Obtained lime powder is confirmed by FT-IR
Surface there is alkoxide layer.The average grain diameter of the lime powder obtained is 0.83 μm, volume density is 0.86g/cm3。
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 C2/ g, 5.6 μm of average grain diameter) and obtain
Lime powder (BET specific surface area 15m2/ g, 5.1 μm of average grain diameter) 3000g and 1-METHYLPYRROLIDONE 105g use content
Product 33L mixer (the New-Gra Machine of SEISHIN ENTERPRISE limited companies manufacture：SEG-350
Type) in equably being mixed under nitrogen environment.Jet mill (SEISHIN is utilized to the lime powder reclaimed from mixer
The STJ-200 types of ENTERPRISE limited companies manufacture) in raw material feed speed 5.0kg/h, crush pressure 0.7MPa's
Under the conditions of carry out pulverization process, obtain the lime powder for the embodiment 2 that particle surface is covered by aprotic polar solvent layer.
During pulverization process, compression fluid is to use nitrogen, and then, reducing mechanism entirety is surrounded with cell (booth), small interior is set to
Nitrogen environment, thus avoids powder and air contact as far as possible.The physical property of the lime powder obtained is shown in table 1.
[embodiment 3]
The amount of 1-METHYLPYRROLIDONE is set to 210g, in addition, manufactured in method same as Example 2,
Obtain the lime powder for the embodiment 3 that particle surface is covered by aprotic polar solvent layer.The lime powder obtained
Physical property be shown in table 1.
[table 1]
Claims (8)
1. a kind of moisture adsorbent, it is made up of powder, and the powder has 0.2~5nm of thickness aprotic polar with surface
The calcium oxide particle of solvent layer is principal component.
2. moisture adsorbent according to claim 1, wherein, the aprotic polar solvent is 1-METHYLPYRROLIDONE.
3. a kind of organic el element moisture adsorbent, it uses moisture adsorbent according to claim 1 or 2.
4. a kind of manufacture method of moisture adsorbent, it is the manufacture method of the moisture adsorbent described in manufacturing claims 1, bag
Include：Dry grinding is carried out in the presence of aprotic polar solvent to calcium oxide.
5. a kind of manufacture method of moisture adsorbent, it is the manufacture method of the moisture adsorbent described in manufacturing claims 1, bag
Include：Calcium oxide is carried out after case of wet attrition in the presence of aprotic polar solvent, separation of solid and liquid and/or drying is carried out.
6. the manufacture method of the moisture adsorbent according to claim 4 or 5, wherein, the aprotic polar solvent is N-
Methyl pyrrolidone.
7. the manufacture method of the moisture adsorbent according to claim 4 or 5, wherein, the moisture adsorbent is organic EL groups
Part is used.
8. the manufacture method of moisture adsorbent according to claim 6, wherein, the moisture adsorbent is organic el element
With.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104994934A CN104994934A (en) | 2015-10-21 |
| CN104994934B true CN104994934B (en) | 2017-08-22 |
Family
ID=51166977
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201480004347.1A Active CN104994934B (en) | 2013-01-10 | 2014-01-08 | Moisture adsorbent and its manufacture method |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP6312439B2 (en) |
| KR (1) | KR102165017B1 (en) |
| CN (1) | CN104994934B (en) |
| TW (1) | TWI618576B (en) |
| WO (1) | WO2014109330A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108698848B (en) * | 2016-02-29 | 2021-09-24 | 宇部材料工业株式会社 | Calcium oxide powder, adsorbent, and method for producing calcium oxide powder |
| JP6603614B2 (en) * | 2016-05-18 | 2019-11-06 | 双葉電子工業株式会社 | Desiccant composition, sealing structure, and organic EL device |
| TWI633525B (en) * | 2016-12-09 | 2018-08-21 | 正文科技股份有限公司 | Parking position sensing device |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1509123A (en) * | 2002-12-04 | 2004-06-30 | ������������ʽ���� | Displaying apparatus and drying agent |
| CN1751085A (en) * | 2003-02-17 | 2006-03-22 | 工程吸气公司 | Composition and devices for gas sorption and process for their manufacturing |
| CN1950299A (en) * | 2004-04-16 | 2007-04-18 | 昭和电工株式会社 | Calcium oxide dispersion liquid and process for production thereof |
| CN103264014A (en) * | 2013-04-22 | 2013-08-28 | 陕西科技大学 | Coating method utilizing organic light-emitting device drying agent which can be coated |
Family Cites Families (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5650115A (en) * | 1979-09-28 | 1981-05-07 | Hiraki Sonoda | Eliminating method for cohesiveness of quick lime powder |
| JPS58180225A (en) * | 1982-04-16 | 1983-10-21 | Adachi Sekkai Kogyo Kk | Surface treatment of quicklime powder |
| JPS6053568A (en) * | 1983-09-02 | 1985-03-27 | Teruo Sasao | Colored slaked lime powder for marking use |
| JPS6163528A (en) * | 1984-09-03 | 1986-04-01 | Shin Etsu Chem Co Ltd | Method for improving fluidity of lime powder |
| JPS61261242A (en) * | 1985-05-15 | 1986-11-19 | 大江化学工業株式会社 | Lime particle |
| JP3385992B2 (en) * | 1999-01-29 | 2003-03-10 | 三浦工業株式会社 | Dioxin decomposition treatment agent and decomposition treatment method |
| JP2006124264A (en) * | 2004-04-16 | 2006-05-18 | Showa Denko Kk | Calcium oxide dispersion liquid and its manufacturing method |
| JP4189390B2 (en) * | 2004-05-14 | 2008-12-03 | 宇部マテリアルズ株式会社 | Method for producing porous slaked lime |
| JP4387870B2 (en) | 2004-05-25 | 2009-12-24 | 宇部マテリアルズ株式会社 | Granular quicklime |
| US8044584B2 (en) * | 2004-11-08 | 2011-10-25 | Samsung Mobile Display Co., Ltd. | Organic electroluminescent device and method for manufacturing the same |
| JP2007035331A (en) * | 2005-07-22 | 2007-02-08 | Optrex Corp | Organic el display panel and water-catching material layer formation device |
| KR101293803B1 (en) * | 2010-11-02 | 2013-08-06 | 주식회사 엘지화학 | Adhesive Film and Encapsulation Method of Organic Electronic Device Using the Same |
| KR20120140394A (en) * | 2011-06-21 | 2012-12-31 | 주식회사 엘지화학 | Adhesive composition for encapsulating an organic electronic element |
-
2014
- 2014-01-08 KR KR1020157021523A patent/KR102165017B1/en active IP Right Grant
- 2014-01-08 JP JP2014001621A patent/JP6312439B2/en active Active
- 2014-01-08 WO PCT/JP2014/050136 patent/WO2014109330A1/en active Application Filing
- 2014-01-08 CN CN201480004347.1A patent/CN104994934B/en active Active
- 2014-01-10 TW TW103100933A patent/TWI618576B/en active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1509123A (en) * | 2002-12-04 | 2004-06-30 | ������������ʽ���� | Displaying apparatus and drying agent |
| CN1751085A (en) * | 2003-02-17 | 2006-03-22 | 工程吸气公司 | Composition and devices for gas sorption and process for their manufacturing |
| CN1950299A (en) * | 2004-04-16 | 2007-04-18 | 昭和电工株式会社 | Calcium oxide dispersion liquid and process for production thereof |
| CN103264014A (en) * | 2013-04-22 | 2013-08-28 | 陕西科技大学 | Coating method utilizing organic light-emitting device drying agent which can be coated |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104994934A (en) | 2015-10-21 |
| TWI618576B (en) | 2018-03-21 |
| WO2014109330A1 (en) | 2014-07-17 |
| JP2014147927A (en) | 2014-08-21 |
| JP6312439B2 (en) | 2018-04-18 |
| TW201434531A (en) | 2014-09-16 |
| KR102165017B1 (en) | 2020-10-13 |
| KR20150106909A (en) | 2015-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US9115033B2 (en) | Moisture absorbent for organic electroluminescence element and production method for same | |
| US8815205B2 (en) | Method for producing spherical alumina powder | |
| US10398652B2 (en) | Sodium bicarbonate particles manufactured by atomization | |
| CN104994934B (en) | Moisture adsorbent and its manufacture method | |
| EP3440016A1 (en) | Getter material comprising intrinsic composite nanoparticles and method of production thereof | |
| US20180236433A1 (en) | Magnesium sulfate-based desiccant and method for producing same | |
| EP2860735A1 (en) | Radioactive material adsorbent, adsorption vessel, adsorption tower, and water treatment device | |
| US20150240040A1 (en) | Calcium carbonate filler for resin, and resin composition containing said filler | |
| US9683104B2 (en) | Surface modification method of calcite | |
| Singh et al. | Utilization of secondary agricultural products for the preparation of value added silica materials and their important applications: a review | |
| JP4387870B2 (en) | Granular quicklime | |
| JP6759327B2 (en) | Calcium oxide powder, adsorbent, and method for producing calcium oxide powder | |
| JP7474221B2 (en) | Manufacturing method of spherical silica powder | |
| JP2003012599A (en) | Powdery potassium acrylate and method for producing the same | |
| JP6484533B2 (en) | Fine strontium carbonate particles | |
| JP2006169062A (en) | Porous particulate containing calcium oxide | |
| JP2018002574A (en) | Manufacturing method of calcium oxide power and calcium oxide power | |
| CN105692682A (en) | Preparation method of environment-friendly zinc oxide particles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |