JPH01246101A - Hydrogen occlusion porous body and production thereof - Google Patents

Abstract

PURPOSE:To make gas permeability and thermal conductivity better and improve absorptivity and purification ability of hydrogen, by mixing a specified powdery alloy with a macromolecular material and forming the mixture. CONSTITUTION:80-97pts.wt. hydrogen occlusion powdery alloy such as Ti-Fe- based alloy with 0.1-200mum particle size are blended with 3-20pts.wt. macromolecular material such as phenolic resin. The resultant mixture is formed into a film shape, etc., to randomly three-dimensionally stacking the hydrogen occlusion alloy powder on top of each other, compound and integrating the mixture with the macromolecular material and form connecting pathways randomly three-dimensionally running therethrough. Thus, the objective H2 occlusion porous body with 20-80vol.% porosity, 0.9-7.5g/cm<2> bulk density and 50mum-5mm thickness, etc., is produced.

Description

DETAILED DESCRIPTION OF THE INVENTION (Industrial Application) The present invention relates to a hydrogen-absorbing porous body made of a hydrogen-absorbing alloy powder and a polymer material, and a method for producing the same.

The hydrogen storage porous body of the present invention can be used in a wide range of fields such as hydrogen separation and purification, hydrogen storage, heat storage material, energy conversion material, etc.

(Conventional technology) Hydrogen energy is a clean energy with few resource constraints and no worries about polluting the natural environment.
It is also easy to store, thermal energy, chemical energy,
It has excellent properties such as a wide range of application fields, such as direct power generation using fuel cells, and in recent years, there has been a lot of interest in the development of utilization technology.

Among the recent developments in hydrogen utilization technology, hydrogen storage alloys in particular have attracted attention as materials that not only transport and store hydrogen, but also have energy conversion functions.For example, Ml-Ni
System, 1. a-Hi system, Ti-Fe-Mn system, Mm
(Mitshu Metal) - Many alloys such as Ni-based alloys have been developed. The properties required of these hydrogen storage alloys vary somewhat depending on the purpose of use, but generally the following properties are required.

(1) Easy activation and large amount of hydrogen absorption.

(2) It has a high hydrogen absorption and release rate and has an appropriate dissociation pressure.

(3) High thermal conductivity.

(4) Even if water is absorbed and released repeatedly, the alloy hardly becomes pulverized.

However, currently developed hydrogen storage alloys
Volume changes occur when hydrogen is absorbed and released, and the repetition of hydrogen absorption and release results in pulverization, which poses a major problem in practice. In other words, the pulverization phenomenon of the alloy places a local load on the container and causes cracks, the pulverized alloy particles clog pipes and valves, and the thermal conductivity decreases, slowing down the absorption and release rate of hydrogen. Various problems occur, such as localized filling of the alloy, uneven heat generation and heat absorption, and temperature unevenness, which are major obstacles to practical application.

(Problems to be Solved by the Invention) The present inventors have completed the present invention as a result of intensive research in order to solve the above-mentioned problems. It is an object of the present invention to provide a hydrogen storage porous body that solves the problems and enables the collection and purification of hydrogen gas and the efficient use of hydrogen energy, and a method for producing the same.

(Means for Solving the Problems) The above objectives are as follows: (A) A large number of hydrogen storage alloy powders with a particle size of 0.1 to 200 μm are randomly overlapped in three dimensions, and are compositely integrated using a polymer material. It has a structure in which (Bl) there are communicating passages that communicate randomly in three dimensions between the large number of hydrogen storage alloy powders, and (C1 hydrogen storage alloy content is 80 to 97%). Hydrogen storage porous body and hydrogen storage alloy powder having a particle size of 0.1 to 200 μm 80
A hydrogen storage porous body characterized by molding a mixture of ~97 parts by weight and 3 to 20 parts by weight of a polymeric material! l! This is achieved through the construction method.

The hydrogen storage alloy powder used in the hydrogen storage porous body of the present invention is not particularly limited, and examples thereof include Ti-Fe-based, ri-p
e-Mn system, Ti-Mn system, Fe-Ti-zr-Nb system, Ti-Co-Mn system, Ti-co-pe system, La-
Ni-based, La-Ni-Al-based, Ca-Ni-based, Mm
(Mitshu Metal) -N i -A / system, Mm-N
i-Fe system, Mm-Ni-Mn system, Mm-Ni system, Lm
(Lanthanum Rich Mitsushi Metal) -Ni series, Lm
-Mn type etc. can be used. Examples of these hydrogen storage alloy compositions include TlFe, T IFe Q,
gMnO,1, TlMn+,5, FeO,94
T 10.96Zr o, o 4Nb O,04+Ti
0oo, 5M, no, 5, T1Co o, 5FeO
, 5, LaNi 5 , LaNi 4. rAl o, a
, 0aNi 5 .

MmNi 4.5Mno, 5. MmNi,s,5A
60.5 etc. These hydrogen storage alloy powders used in the present invention usually have an average particle size of 0.1 to 200μ.
ITI, preferably having an average particle size of 1 to 100 μm, most preferably 5 to 60 μm. If the average particle size is too small, it is difficult to form communication passages of uniform size randomly between the alloy powder particles to obtain a porous body with good gas permeability. Furthermore, if the average particle size of the hydrogen-absorbing alloy powder is too large, the uniformity of the hydrogen-absorbing porous body of the present invention will deteriorate, the shape retention will decrease, and cracks will occur due to repeated hydrogen absorption and release. It becomes difficult to prevent the occurrence of

The polymeric materials used in the present invention include phenolic resin,
Thermosetting resin selected from melamine resin, urea resin, epoxy resin, furan resin, etc., or polyamide resin, polyester resin, polyethylene resin, polypropylene resin, polystyrene resin, acrylic resin, vinyl chloride IU! , a thermoplastic resin selected from fluororesins, polyacetal resins, polycarbonate resins, polyurethane resins, etc., or polyvinyl alcohol resins, or a mixture of two or more thereof can be used.

Examples of the thermosetting phenolic resin include resol resin and novolac resin. Resole resin is an initial product obtained by reacting phenols with aldehydes in the presence of a basic catalyst, and is usually a self-thermal crosslinking phenol resin with a molecular weight of about 600 or less, rich in methylol groups, and methanol Although it is often used as a liquid resin using acetone as a solvent, it is an initial condensate made by reacting 1.5 to 3.5 moles of aldehydes with 1 mole of phenol in the presence of a slightly excess alkali catalyst. It can also be made into a water-soluble resol resin by keeping it in a stable water-soluble state. As a curing catalyst for accelerating the curing of the resol resin, inorganic acids such as sulfuric acid and hydrochloric acid, or organic acids such as oxalic acid, acetic acid, para-toluenesulfonic acid, maleic acid and malonic acid can be used. Novolac resin is prepared by adding, for example, oxalic acid, formic acid,
It is obtained by reacting in the presence of an acid catalyst such as hydrochloric acid, and is itself a thermoplastic resin, but for example,
It can be cured by adding bexamethylenetetramine (hexamine) and causing a heating reaction.

Melamine resin and urea resin are initial condensates of melamine-formaldehyde and urea-formaldehyde, respectively, and are water-soluble. Curing agents for melamine resins and urea resins include inorganic acids such as hydrochloric acid and sulfuric acid, esters of carboxylic acids such as dimethyl oxalate, and amine hydrochlorides such as ethylamine hydrochloride and triethanolamine hydrochloride. can be used.

The most common epoxy resin is a condensation product of bisphenol A and epichlorohydrin, but phenolic compounds such as novolac may be used instead of bisphenol A, or unsaturated compounds such as cyclopentadiene or cyclohexene may be used. , or polybutadiene, in which an epoxy group is introduced into an unsaturated group using an organic peracid, may also be used. As the curing agent for the epoxy resin, an amine type or an organic acid anhydride type can be used.

The amine type curing agent is a room temperature or medium temperature curing agent, and aliphatic polyamines such as diethylenetriamine and triethylenetetramine, aromatic polyamines such as metaphenylenediamine and diaminodiphenylmethane are suitable. Suitable organic acid anhydride curing agents include phthalic anhydride, hexahydrophthalic anhydride, methyltetrahydrophthalic anhydride, and the like.

Furan resins include furifuryl alcohol resin, furifuryl alcohol phenol resin, furifural resin,
Examples include furifural phenol resin and furifural ketone resin. As a curing agent for these resins, for example, organic acids such as aniline hydrochloride and para-toluenesulfonic acid can be used.

Examples of thermoplastic polyamide resins include polycaproamide (6-nylon), polyhexamethylene adipamide (6,6-nylon), polyhexamethylene sebacamide (6,10-nylon), etc. Preferably used.

As the polyester resin, a saturated polyester resin is preferable, and for example, polyethylene terephthalate, polytetramethylene terephthalate, polyhexamethylene terephthalate, etc. are preferably used.

Contains 85% by weight or more. The polypropylene resin preferably contains propylene units in the polymer chain in an amount of 50% by weight or more, more preferably 85% by weight or more.

The acrylic resin preferably contains 50% by weight or more, more preferably 85% by weight or more of units of methyl or ethyl ester of acrylic acid or methacrylic acid in the polymer chain.

In the vinyl chloride resin, vinyl monomer units having ethylenically unsaturated bonds are contained in the polymer chain in an amount of preferably 50% by weight or more, more preferably 85% by weight or more.

The fluororesin preferably contains 50% by weight or more, more preferably 85% by weight or more of units of fluorine-containing vinyl monomers such as tetrafluoroethylene, fluoroethylene, and hexafluoropropylene in the polymer chain.

A polyurethane resin is obtained by mixing a polyisocyanate and a polyol together with a catalyst and reacting the mixture.

As the polyisocyanate, for example, tolylene diisocyanate (TDI), diphenylmethane diisocyanate (MDI) or modified MDI can be used. Polyols include polyether compounds and polyester compounds. Polyether compounds are the addition polymerization of ethylene oxide or propylene oxide to polyhydric alcohols such as glycerin, sorbitol, trimethylpropane, and sucrose. Polyester compounds are , adipic acid, phthalic anhydride, dimer acid, and other polyvalent acid polyhydric alcohols. As the catalyst used for the reaction between polyisocyanate and polyol, amine compounds such as triethylenediamine, NN-dimethylcyclohexylamine, and trimethylpiperazine, and organometallic compounds such as stannath octoate and dibutyltin laurate can be used.

Polyvinyl alcohol-based resins refer to polyvinyl alcohol and polyvinyl acetal resins such as polyvinyl formal and polyvinyl benzal, which are obtained by mixing polyvinyl alcohol and aldehydes as crosslinking agents with an acid catalyst and reacting the mixture.

A large number of hydrogen-absorbing alloy powders having a particle size of 01 to 200 μm are three-dimensionally randomly overlapped and have a structure in which they are combined by the above-mentioned polymeric material. This structure in which a large number of hydrogen-absorbing alloy powders are three-dimensionally randomly overlapped and combined by a polymer material is shown in Figures 1-1al and (bl, Figure 2-11).
, can be confirmed by the scanning electron micrograph in (b).

Figure 1- (a) and (b) show Ca as hydrogen storage alloy powder.
This is a scanning electron micrograph of a cross section of a hydrogen storage porous body formed into a film using Ni5 powder and polyvinyl alcohol as a polymer material. The content of hydrogen storage alloy powder in the hydrogen storage porous body is 95% by weight. Figure 2
-(a) and (b) are CaNi as hydrogen storage alloy powder.
5 is a scanning electron micrograph of a cross section of a hydrogen storage porous body formed into a columnar shape using powder and phenol resin as a polymer material.

The hydrogen storage alloy content in the hydrogen storage porous body is 91% by weight.

In these photographs, it can be seen that a large number of hydrogen-absorbing alloy powders overlap in a three-dimensional random manner, and that communication passages that run three-dimensionally at random exist between them.

Hydrogen storage alloy powder in the hydrogen storage porous body of the present invention,
The content ratio of the polymer material is 80 to 9% of the hydrogen storage alloy powder.
7% by weight, and 3-20% by weight of polymeric material.

The content of this hydrogen storage alloy powder is preferably 83 to 9
6% by weight, most preferably 85-95% by weight.

When the content of the hydrogen-absorbing alloy powder is small, the hydrogen-absorbing and storage capacity of the hydrogen-absorbing porous body of the present invention decreases, and the hydrogen-absorbing rate of spring core semi-hydrogen also decreases.

Further, the thermal conductivity of the hydrogen storage porous body also decreases. If the content of the hydrogen-absorbing alloy powder is too large, the bonding force through the polymer material that binds the hydrogen-absorbing alloy powder and coalesces decreases, and the shape retention of the hydrogen-absorbing porous body decreases. The strength decreases and the porous body is damaged due to repeated absorption and release of hydrogen.

The diameter of the communication passages running randomly in three dimensions between the large number of hydrogen storage alloy powders in the hydrogen storage porous body is preferably:
0.1 to 100 μm, most preferably 0.5 to 100 μm
It is 50 μm. After the hydrogen stored in the hydrogen storage porous body of the present invention enters the communication passage inside the porous body from the outside,
It reaches the surface of the hydrogen storage alloy powder particles and is occluded within the particles. Therefore, it is preferable that the communication passages between the alloy powders are randomly distributed with variable pore diameters.

The porosity of the hydrogen storage porous material of the present invention is preferably 20 to 20.
80% by volume, most preferably 80-60% by volume.

Further, the bulk density is preferably 0.9 to 7,517 cm8
, most preferably 1.0 to 5.017 cm".

There is no particular restriction on the shape of the hydrogen storage porous body of the present invention,
It can take various forms such as cylinders, cylinders, blocks, pellets, sheets, and films.

In particular, film-like or sheet-like hydrogen storage porous materials with a thickness of 50 μm to 5 mm have high functionality not found in conventional hydrogen storage alloys, and are used in a wide range of fields such as hydrogen separation and purification membranes, electrode materials, and energy conversion materials. It becomes possible to use it for

The hydrogen storage porous body of the present invention comprises 80 to 97 parts by weight of hydrogen storage alloy powder with a particle size of 0.1 to 200 μm and 3 to 2 parts by weight of a polymeric material.
0 parts by weight of the mixture can be produced by molding.

When a thermosetting resin is used as the polymer material, liquid or powdered phenol resin, melamine resin, area resin, epoxy resin, furan resin, etc. can be used. In particular, phenol resins, melamine resins, and area resins are preferred because they are easy to handle and have good moldability.

When using hydrogen storage porous resin, the thermosetting resin is dissolved in water or a solvent to make it liquid, then mixed with hydrogen storage alloy powder, formed into a predetermined shape such as a block, plate, film, etc., and hardened to form a hydrogen storage porous resin. You can get a body. Further, a porous hydrogen storage body can be obtained by using a powdered initial condensate as the thermosetting resin, mixing it with a predetermined amount of hydrogen storage alloy powder, and performing a curing reaction.

When using a thermoplastic resin as a polymeric material, the thermoplastic resin in powder or pellet form and hydrogen storage alloy powder should be mixed in a predetermined ratio and then molded at a temperature equal to or higher than the softening point of the thermoplastic resin. A hydrogen storage porous body can be obtained by this method.

In addition, when polyvinyl alcohol-based tree d is used as a polymer material, polyvinyl alcohol is dissolved in hot water to form an aqueous solution of a predetermined concentration, and then mixed with hydrogen-absorbing alloy powder and molded to form a hydrogen-absorbing porous material. It can be done.

Furthermore, polyvinyl acetal resins such as polyvinyl formal and polyvinyl benzal can also be produced by mixing polyvinyl alcohol with its crosslinking agent aldehyde and acid catalyst and reacting the mixture.

For example, dissolve a predetermined amount of polyvinyl alcohol in warm water, add a pore-forming material such as starch if necessary and mix evenly, add a predetermined amount of hydrogen storage alloy powder, mix thoroughly, and then add a crosslinking agent. A hydrogen-absorbing porous body can be obtained by adding an appropriate amount of formalin and sulfuric acid as an acid catalyst and carrying out a curing reaction at a temperature of about 40 to 80°C in a frame of a desired shape.

Molding methods for producing the hydrogen-absorbing porous body of the present invention from the above-mentioned polymeric material and hydrogen-absorbing alloy powder include a casting method, an extrusion molding method, and an injection molding method in which a slurry-like mixture is hardened and reacted in a mold. , a doctor blade method, a hot press method, etc. can be used.

(Effect of the invention) The hydrogen storage porous material of the present invention has excellent shape retention,
It will not be damaged even after repeated hydrogen absorption and release.
Various problems caused by pulverization, which is a major hindrance in practical use of hydrogen-absorbing porous materials, can be solved. In addition, the hydrogen storage porous body has a large number of hydrogen storage alloy powders having a particle size of 0.1 to 200 μm overlapping each other in a three-dimensional random manner, and communication passages that run randomly in three dimensions between the alloy powders. It has good gas permeability and uniform thermal conductivity, has a high hydrogen gas storage and release rate, and has uniform heat absorption and heat generation due to storage and release, and does not cause local heat accumulation.

The hydrogen storage porous body of the present invention having such characteristics can be used for hydrogen separation and purification, hydrogen storage, or as a heat storage material for heat pumps, in exhaust heat heating and cooling systems, horticultural heat pumps, and the like.

Example 1 Water was added to polyvinyl alcohol having a degree of polymerization of 1700 and a degree of saponification of 99%, and the mixture was heated and dissolved to obtain a 1Qwt% polyvinyl alcohol aqueous solution. On the other hand, bulky hydrogen storage alloy Ca
Ni5 was ground with a ball mill to give an average particle size of 46
A hydrogen storage alloy powder of μm size was prepared. This CaNi5
The powder and polyvinyl alcohol aqueous solution were mixed at a predetermined ratio, formed into a film using a doctor blade on a glass plate, and then dried in a dryer at 60°C for 24 hours to form a film-like hydrogen storage porous film with a thickness of approximately 200 tim. I got a body.

Table 1 shows the composition and basic physical properties of the obtained film-like hydrogen storage porous material.

Table 1 Among the above samples, 1 and 2 had good shape retention and excellent sinterability. However, in Sample 8, the ability to support the alloy was poor, and the alloy powder fell off when deformed.

Regarding Samples 1 and 2, hydrogen storage and release were repeatedly measured using the hydrogen storage property measuring device shown in FIG. 8, and pressure-composition isotherms (PCT lines) were measured. Also, P
The internal structure of the hydrogen storage porous material before and after the TC line measurement was examined using a scanning electron microscope.

Figure '(a) + ('bl Shows photographs of sample 2 before and after the hydrogen absorption experiment (POT line measurement) and - times.

Figure 1-(From al(bl), the hydrogen storage porous material of the present invention is
It can be confirmed that a large number of hydrogen-absorbing alloy powders have a three-dimensionally randomly overlapped and combined structure. Further, the average diameter of continuous passages between a large number of hydrogen storage alloy powders was 2.5 μm. In addition, in the sample shown in Figure 1-(b) after one hydrogen storage test, cracks occurred in the alloy powder and it became finely powdered, but these powders were It was supported within the original skeletal structure and no shedding was observed. Furthermore, for sample 2, after repeating hydrogen absorption and desorption 20 times, the cross section of the sample was observed using a scanning electron microscope. Although the powder was finely ground, almost no dropout was observed. .

Next, a PTO diagram measured using Sample 1 is shown in FIG.

From Figure 4, the plateau pressure is lower on both the occlusion side and the dissociation side than in the case of the alloy alone, but the maximum occlusion amount is due to the atomic ratio (H/M: L (= hydrogen, M = hydrogen storage alloy) 0 It can be seen that the shape of the PCT wire is not significantly different from that when the alloy is used alone.

Example 2 Spherical phenolic resin powder with an average particle size of about 20 μm (Kanebo Co., Ltd.)
..., product name: Bell Pearl 几-800) and water-soluble resol resin (Showa Kobunshi ■ product, product name: Nijiyounol BR)
, L-2854, solid content concentration 60% by weight) at a weight ratio of 2
Mixed at 0:80.

Furthermore, this mixed solution and hydrogen storage alloy powder crushed to an average particle size of 58 μm were mixed at a predetermined ratio, and after casting into a mold, the phenol resin was cured at 80°C for 24 hours to form a cylindrical shape with a diameter of 16 m x 150 mm. A hydrogen storage porous body was manufactured.

The composition and basic physical properties of the obtained hydrogen storage porous body are shown in Table 2.

Table 2 Among the above samples, 4 and 5 showed good shape retention. In sample 6, the bonding strength between the alloy particles was weak and did not maintain sufficient strength for practical use.

Figure 2-(a) shows hydrogen absorption experiment of sample 5 (POT line measurement)
The previous scanning electron micrograph is also shown as a photograph after PCT line measurement was performed once on 2-(bl. Furthermore, Figure 5 shows the measured POT diagram. Figure 2-(al (bl It can be confirmed that the sample of Example 2 also has a structure in which a large number of hydrogen-absorbing alloy powders are three-dimensionally randomly overlapped and coalesced, similar to the case of Example 1. The storage experiment was repeated 20 times in the same manner as in Example 1, but almost no alloy powder was observed to fall off, and there was no decrease in the amount of hydrogen storage.

Example 3 Water-soluble melamine resin (Sumitomo Chemical Co., Ltd. (candle products, Sumitex Resin M-8, solid content concentration 80% by weight) 100y and hydrogen storage alloy powder LaNi15 (average particle size 53 μm)
) 800y was mixed and then molded into a plate shape of 10th order of thickness. 5f of a curing agent (Sumitex Resin ACX) was added to the water-soluble melamine resin in advance, and the plate-shaped molded body was heat-treated at 60°C for 24 hours to obtain a hydrogen-absorbing porous body.

The content of LaNi5 alloy powder in the hydrogen storage porous body was 90% by weight, the bulk density was 2.0497 cm8, the average pore diameter was 88 m, and the porosity was 78%. As in Examples 1 and 2, the hydrogen-absorbing porous body was found to have a structure in which a large number of hydrogen-absorbing alloy powders were randomly overlapped in three dimensions and were combined by a polymer material, as in Examples 1 and 2. It was confirmed that it had sufficient shape retention.

Example 4 2 rrsmi x 6 mmL of chip-shaped 6 nylon resin (Kanebo Co., Ltd., manufactured by Koshi, MCMC-10OL) 1, hydrogen storage alloy powder with an average particle size of 24 μm, and 9 kg of TiFe
The mixture was sufficiently stirred and mixed in a mixer kept at 220 to 280°C, and then extruded through a slit-shaped nozzle with a thickness of 4 mm to obtain a hydrogen storage porous body with a thickness of about 4 mm.

The hydrogen storage porous body had a bulk density of 8.02 F/cm8, an average pore diameter of 2 μm, and a porosity of 49%.

By observing the internal structure of the hydrogen-absorbing porous body using a scanning electron microscope, it was confirmed that the hydrogen-absorbing porous body has a structure in which a large number of hydrogen-absorbing alloys overlap in a three-dimensional random manner and are combined with a polymeric material. It also had sufficient shape retention.

[Brief explanation of the drawing]

Figure 1 shows a hydrogen-absorbing porous body formed into a film using CaNi5 powder as a hydrogen-absorbing alloy powder and polyvinyl alcohol as a polymer material. (a) is before hydrogen absorption, and (b) is after one hydrogen absorption. It is a scanning electron micrograph showing a cross-sectional structure. Figure 2 shows a hydrogen-absorbing porous body formed into a cylinder using CaNi5 powder as a hydrogen-absorbing alloy powder and phenol resin as a polymer material, (a) before hydrogen absorption, fb
) is a scanning m-son micrograph showing the cross-sectional structure after one hydrogen absorption. Figure 3 is a diagram of the hydrogen storage property measuring device, in which (1) is a constant temperature water tank, (2) is a sample container, (3) is a sample, (4) is a vacuum pump, (5) is a hydrogen storage tank, and (6) is a sample container. ) is a pressure sensor, (7) is a recorder, (8) is a hydrogen cylinder, (
9) to α1 are valves, (14 is a hydrogen introduction pipe. FIGS. 4 and 5 are P of the hydrogen storage porous body according to the present invention.
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Claims (1)

[Claims] (1) (A) It has a structure in which a large number of hydrogen storage alloy powders with an average particle size of 0.1 to 200 μm are randomly overlapped in three dimensions and are compositely integrated with a polymer material, (B) The hydrogen A hydrogen storage porous body (2) characterized in that there are three-dimensionally random communication passages between the storage alloy powders, and (C) the hydrogen storage alloy content is 80 to 97% by weight. ) Particle size 0.1-2
1. A method for producing a hydrogen-absorbing porous body, which comprises molding a mixture of 80 to 97 parts by weight of a hydrogen-absorbing alloy powder having a diameter of 00 μm and 3 to 20 parts by weight of a polymeric material.