JPH02252642A - Hardener for alkali silicate and treating agent for inorganic fibrous material containing thereof - Google Patents
Hardener for alkali silicate and treating agent for inorganic fibrous material containing thereofInfo
- Publication number
- JPH02252642A JPH02252642A JP7069489A JP7069489A JPH02252642A JP H02252642 A JPH02252642 A JP H02252642A JP 7069489 A JP7069489 A JP 7069489A JP 7069489 A JP7069489 A JP 7069489A JP H02252642 A JPH02252642 A JP H02252642A
- Authority
- JP
- Japan
- Prior art keywords
- alkali silicate
- acid
- alkali
- hardener
- water
- 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.)
- Granted
Links
- 229910052910 alkali metal silicate Inorganic materials 0.000 title claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 title claims description 32
- 239000004848 polyfunctional curative Substances 0.000 title abstract description 5
- 239000002657 fibrous material Substances 0.000 title description 2
- 239000002253 acid Substances 0.000 claims abstract description 20
- -1 alkylene carbonate Chemical compound 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 13
- 150000004645 aluminates Chemical class 0.000 claims abstract description 11
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims abstract description 8
- 150000001299 aldehydes Chemical class 0.000 claims abstract description 8
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229940015043 glyoxal Drugs 0.000 claims abstract description 5
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 3
- HXDLWJWIAHWIKI-UHFFFAOYSA-N 2-hydroxyethyl acetate Chemical compound CC(=O)OCCO HXDLWJWIAHWIKI-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000007795 chemical reaction product Substances 0.000 claims abstract 2
- 239000012784 inorganic fiber Substances 0.000 claims description 4
- 150000001242 acetic acid derivatives Chemical class 0.000 claims description 3
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 2
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 2
- 239000000600 sorbitol Substances 0.000 claims description 2
- XYAUIVRRMJYYHR-UHFFFAOYSA-N acetic acid;propane-1,2,3-triol Chemical compound CC(O)=O.OCC(O)CO XYAUIVRRMJYYHR-UHFFFAOYSA-N 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 abstract description 18
- 239000007864 aqueous solution Substances 0.000 abstract description 13
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 229910001388 sodium aluminate Inorganic materials 0.000 abstract description 4
- 239000010425 asbestos Substances 0.000 description 16
- 229910052895 riebeckite Inorganic materials 0.000 description 16
- 239000007788 liquid Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 239000000835 fiber Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000000243 solution Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000004111 Potassium silicate Substances 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 description 3
- 229910052913 potassium silicate Inorganic materials 0.000 description 3
- 235000019353 potassium silicate Nutrition 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000011490 mineral wool Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- KVOIJEARBNBHHP-UHFFFAOYSA-N potassium;oxido(oxo)alumane Chemical compound [K+].[O-][Al]=O KVOIJEARBNBHHP-UHFFFAOYSA-N 0.000 description 2
- 150000004760 silicates Chemical class 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 239000011975 tartaric acid Substances 0.000 description 2
- 235000002906 tartaric acid Nutrition 0.000 description 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WSMYVTOQOOLQHP-UHFFFAOYSA-N Malondialdehyde Chemical compound O=CCC=O WSMYVTOQOOLQHP-UHFFFAOYSA-N 0.000 description 1
- 229920001744 Polyaldehyde Polymers 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- QLVHFTGKDGTJDH-UHFFFAOYSA-N acetic acid;ethenyl acetate Chemical compound CC(O)=O.CC(=O)OC=C QLVHFTGKDGTJDH-UHFFFAOYSA-N 0.000 description 1
- 150000001243 acetic acids Chemical class 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008119 colloidal silica Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- LDHQCZJRKDOVOX-NSCUHMNNSA-N crotonic acid Chemical compound C\C=C\C(O)=O LDHQCZJRKDOVOX-NSCUHMNNSA-N 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920006332 epoxy adhesive Polymers 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011440 grout Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- PAZHGORSDKKUPI-UHFFFAOYSA-N lithium metasilicate Chemical compound [Li+].[Li+].[O-][Si]([O-])=O PAZHGORSDKKUPI-UHFFFAOYSA-N 0.000 description 1
- 229910052912 lithium silicate Inorganic materials 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 229940118019 malondialdehyde Drugs 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000002940 repellent Effects 0.000 description 1
- 102220175917 rs375609763 Human genes 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010454 slate Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B20/00—Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
- C04B20/10—Coating or impregnating
- C04B20/1055—Coating or impregnating with inorganic materials
- C04B20/1074—Silicates, e.g. glass
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/04—Carboxylic acids; Salts, anhydrides or esters thereof
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Aftertreatments Of Artificial And Natural Stones (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
Description
【発明の詳細な説明】
〈産業上の利用分野〉
本願発明は、珪酸アルカリ用硬化剤、それを含有するア
スベスト、ロックウール等の無ｎ繊維貿の接着、難燃化
、固化、表面硬化等の処理剤に関するものである。[Detailed Description of the Invention] <Industrial Field of Application> The present invention is applicable to curing agents for alkali silicate, adhesion, flame retardation, solidification, surface curing, etc. of non-n fibers such as asbestos and rock wool containing the same. The present invention relates to a processing agent.
〈従来の技術〉
従来より、アスベスト、ロックウール等の照ｎ繊維質の
処理には、水溶性高分子、水分散樹脂等の有機接肴剤が
使用されているが、これらのものは無Ｗ１［質の湿潤除
去の目的には適用できるが、除去せずに固化の目的では
、耐火、防火、防煙の問題があり使用しり１い。又、無
機系のものでは珪酸アルカリ水溶液やコロイダルシリカ
の使用が試みられているが、これらは乾燥までの間に水
の移動と共に溶質成分が一乾燥表面へ移ｖＪｖる、所謂
マイクレージョン現染を起こし、表面のみが堅く、内部
は柔らかい不均一な固化になる問題がある。<Conventional technology> Conventionally, organic adhesives such as water-soluble polymers and water-dispersed resins have been used to treat fibrous materials such as asbestos and rock wool. [It can be applied for the purpose of removing moisture, but it cannot be used for the purpose of solidifying without removing it because of problems with fire resistance, fire prevention, and smoke prevention. In addition, attempts have been made to use alkali silicate aqueous solutions and colloidal silica for inorganic products, but these are known to cause so-called microclision dyeing, in which solute components migrate to the drying surface along with the movement of water during drying. The problem is that only the surface becomes hard and the inside becomes soft and unevenly solidified.
珪酸塩類のこの問題は、珪酸アルカリ用硬化剤を使用し
て乾燥前に珪酸塩の固定を行なうことによって回避する
ことができる。硬化剤には、粉末状のものと水溶液状の
ものがあるが、粉末状のものは無機繊維質表面で濾過さ
れて内部へ浸入しないので使用出来ない。水溶液状のも
のは硬化時間が短いものが一般的であり、アスベスト処
理の様に１時間−ｖＩＶｆ間の作業に合せて硬化時聞く
所謂ポットライフ）を長くとれるものはない。This problem with silicates can be avoided by fixing the silicates before drying using an alkali silicate hardener. There are two types of curing agents: powdered ones and aqueous solutions, but powdered ones cannot be used because they are filtered through the inorganic fibrous surface and do not penetrate into the interior. Aqueous solutions generally have a short curing time, and there is no such thing as asbestos treatment, which has a long curing time (the so-called pot life) that can be used for 1 hour to vIVf.
また、水溶液状の珪酸アルカリ用硬化剤としては■無機
塩又はａ機酸水溶液、■有機酸又番ま有機酸１スプルが
実用されている。As aqueous solutions of curing agents for alkali silicate, (1) inorganic salt or organic acid aqueous solution, (2) organic acid or organic acid 1 sprue are in practical use.
しかしながら、■は硬化時間の調節が難しく、又、低強
度の硬化体しか得られず、特に硬化時間を数時間とした
場合には適用できない。However, method (2) is difficult to control the curing time, and only a cured product with low strength can be obtained, so it cannot be applied especially when the curing time is several hours.
■の有機酸を用いた場合は■と同様であるが、有機酸エ
ステルを用いた場合は硬化時間が数１０分の場合には比
較的強度のおる硬化体を得ることができるが、硬化時間
を１時間以上にづると強度不だのものしか青られない。When an organic acid is used in (2), it is the same as (2), but when an organic acid ester is used, a relatively strong cured product can be obtained if the curing time is several tens of minutes, but the curing time is If it lasts for more than 1 hour, only those with poor strength will be able to be blued.
又、例えば、特開昭５１−５５１１２号公報にはＪ１酸
ソーダとアルミン酸ソータとクエン酸又は酒石酸の混合
物かグラウト剤として提案されているか、この組成物で
硬化時間を６０分としたときには、強度が低いものしか
得られず、硬化時間は３０分以下か限界であつ【、それ
以上では硬化体かゼリー状どイより実用に供せない。こ
の様な組成物をアスベスト等の無機繊Ｎ賀処理用に使用
ｊうど固化性能を発揮しないばかりか、乾燥物が粉化し
て逆に粉塵発生源となるａブそれがある。For example, in JP-A-51-55112, a mixture of sodium J1 acid, sorta aluminate acid, and citric acid or tartaric acid is proposed as a grout agent, and when this composition is used for a curing time of 60 minutes, Only a product with low strength can be obtained, and the curing time is limited to 30 minutes or less, and if it is longer than that, the product becomes a cured product or a jelly-like product, and cannot be used for practical purposes. When such a composition is used to treat inorganic fibers such as asbestos, it not only does not exhibit solidifying performance, but also causes the dried material to become powder and become a source of dust.
く光明が解決しようとする課題〉
Ｊ１酸アルカリを１時間〜数時間という硬化時間を有し
、且つ高強度の硬化体が得られるアスベスト等の無ａｍ
維質の飛散防止等の処理剤として有効なものにプること
が課題である。Problems that Kukomei is trying to solve〉 J1 acid alkali has a curing time of 1 hour to several hours, and a high-strength cured product can be obtained without am asbestos etc.
The challenge is to find an effective treatment agent for preventing fiber scattering.
そこで本光明者は鋭意？ｉｌｆ究を行なった結果本梵明
を得た。So, is this Komyosha diligent? As a result of studying ILF, I obtained this Brahma.
ぐ８￥Ａを解決するだめの１段〉
即ち、本発明は、アルデヒド類、水溶性低級アルキレン
カーボネート及び多価アルコール酢酸エステルから選ば
れた１種以上、及びオキシカルボン酸アルミニウム錯体
を含有してなるＪ土酸アルｈり用硬化剤である。One step to solving the problem 8 A> That is, the present invention contains one or more selected from aldehydes, water-soluble lower alkylene carbonates, and polyhydric alcohol acetate esters, and an aluminum oxycarboxylic acid complex. This is a curing agent for J soil acid alkali.
ここで、アルデヒド類とは水訂竹のホルムアルｆごド、
アセトアルデヒド等のｔノアルデヒドやグリオキザール
、マロンジアルデヒド等のポリアルデヒド等であり、特
に硬化時間の調節にはグリオキザールが好ましい。Here, the aldehydes are Suiseitake's formal f.
These include t-aldehydes such as acetaldehyde, polyaldehydes such as glyoxal and malondialdehyde, and glyoxal is particularly preferred for adjusting the curing time.
水溜性低級アルキレンカーボネートとしては、■チレン
カーボネート、プロピレンカーボネート等が挙げられる
。Examples of water-retaining lower alkylene carbonates include ethylene carbonate, propylene carbonate, and the like.
多価アルコール酢酸ニスミルとしては、エチ１／ングリ
コール酢酸ニスデル、グリセリン酢酸ニス７−ル、ソル
ビト−ル酢酸エステル等があるが、特にエチレングリコ
ールジアセデ−１・が好ましい。Examples of the polyhydric alcohol nisyl acetate include ethyl 1/glycol nysyl acetate, glyceryl nysyl acetate, and sorbitol acetate, with ethylene glycol diacetate being particularly preferred.
又、オキシカルボン酸アルミニウム錯体は、一般にはオ
キシカルボン酸とアルミン酸アルカリ水溶液との反応に
よる生成物が使用される。Further, as the aluminum oxycarboxylic acid complex, a product obtained by reacting an oxycarboxylic acid with an aqueous alkali aluminate solution is generally used.
ここで゛、オキシカルボン酸としてはりＪン酸、乳酸、
グリコール酸、リンゴ酸、酒石酸、グ耐−コン酎、クロ
トン酸等からなる群より選ばれた１梯又は２種以上が挙
げられるが、クエン酸が特に好ましい。Here, the oxycarboxylic acids are phosphoric acid, lactic acid,
Examples include one or more selected from the group consisting of glycolic acid, malic acid, tartaric acid, glutinous acid, crotonic acid, etc., and citric acid is particularly preferred.
アルミン酸アルカリとして番よアルミン酸アルカリウム
、アルミン酎カリウム水溶液等か挙げられるが、アルミ
ン酸すトリウムが特に好ましい。Examples of the alkali aluminate include alkaline potassium aluminate, aqueous potassium aluminate solution, etc., and sodium aluminate is particularly preferred.
本発明の珪酸アルカリ用硬化Ｒ口よ以上の成分比を右す
−る。The curing ratio for the alkali silicate of the present invention is determined by the above component ratios.
硬化剤を水溶液の形で金弟を１００％とすると、アルミ
ン酸アルカリ水溶液は、一般に３０〜４ ｏ ％固形３
７の水溶液であるが、全量に対して０．２〜５．０％を
含有し、好ましくは０．５〜３．０％を含有する。その
理由は、５．０％を超えると硬化時間が短くなりすぎ目
的とするものが得られず、０．２％未満では強度のない
ものしか得ら−ｈないからである。If the curing agent is in the form of an aqueous solution and the hardening agent is 100% solid, the alkali aluminate aqueous solution generally has a solid content of 30 to 4 o%.
The aqueous solution of No. 7 contains 0.2 to 5.0%, preferably 0.5 to 3.0%, based on the total amount. The reason is that if it exceeds 5.0%, the curing time becomes too short and the desired product cannot be obtained, and if it is less than 0.2%, only a product with no strength can be obtained.
オキシカルボンｉ！は、その分子Φによって異なるので
一概に言うことはてきないが、おおむね０．０１〜３０
％であり、例えば、クエン酸（分子１２１０）では、全
量に対して０．１〜３．５％を含有し、好ましくは０．
３〜２．０％である。アルミン酸アルカリのアルミニウ
ムイオンをキレート化するには当量以上のオキシカルボ
ン酸が必要であり且つ、アルミン酸アルカリのアルカリ
を中和してｐＨ３〜９にする帛のオキシカルボン酸が必
要となる。従って、アルミン酸アルカリの含有量によっ
て必然的にオキシカルボン酸の巾は決る。Oxycarbon i! cannot be generalized because it varies depending on the molecule Φ, but it is approximately 0.01 to 30
%, and for example, citric acid (molecule 1210) contains 0.1 to 3.5% based on the total amount, preferably 0.
It is 3 to 2.0%. In order to chelate the aluminum ion of the alkali aluminate, an equivalent or more amount of oxycarboxylic acid is required, and a large amount of oxycarboxylic acid is required to neutralize the alkali of the alkali aluminate to pH 3 to 9. Therefore, the width of the oxycarboxylic acid is necessarily determined by the alkali aluminate content.
又、アルデヒド類、水溶性低級アルキレンカーボネート
及び多価アルコール酢酸から選は“れた１種以上は珪酸
アルカリの種類によって責なるが、おおむね２〜１０％
を含有し、好ましくは３〜８％である。その理由は１０
％を超えると硬化時間が早すきて目的に合わず、２％未
満では硬化時間が必要以上に長くなり意味がないからで
ある。In addition, one or more selected from aldehydes, water-soluble lower alkylene carbonates, and polyhydric alcohol acetic acids are responsible depending on the type of alkali silicate, but generally 2 to 10%.
and preferably 3 to 8%. The reasons are 10
This is because if it exceeds 2%, the curing time becomes too fast and is not suitable for the purpose, and if it is less than 2%, the curing time becomes longer than necessary and is meaningless.
本光明の珪酸アルカリ用硬化剤は以下の方法によって調
製することが出来る。The curing agent for alkali silicate according to the present invention can be prepared by the following method.
まず、アルミン酸アルカリとオキシカルボン酸の混合を
行なう。この混合は中和反応でありｔ）Ｈ３−９とする
。そのためには、アルミン酸アルカリ溶液中の苛性アル
カリ１グラム当吊に対してオキシカルボン酸を０．５〜
２グラム当串が適当である。こうして１＃られる液は透
明であり、オキシカルボン酸のキレ−１′−効果により
安定に貯蔵できる。次いで、これにアルデヒド類、水溶
性低級アルキレンカーボネート及び多価アルコール酢酸
エステルから選ばれた１種以上を加えるが、その添加量
は硬化時間を決定することになり任意にきめることがで
きるが、実用的な範囲としては■１酸アルカリ溶液のア
ルカリ成分１グラム当最に対して０．００１〜１グラム
当塁である。こうしてに号られる液は透明であり安定に
貯蔵できる。First, alkali aluminate and oxycarboxylic acid are mixed. This mixing is a neutralization reaction and is referred to as t) H3-9. To do this, add 0.5 to 0.5 to 0.5 to 1 g of oxycarboxylic acid per 1 gram of caustic alkali in an alkaline aluminate solution.
A 2 gram skewer is appropriate. The liquid thus prepared is transparent and can be stored stably due to the clear-1'-effect of the oxycarboxylic acid. Next, one or more selected from aldehydes, water-soluble lower alkylene carbonates, and polyhydric alcohol acetates are added to this, but the amount added will determine the curing time and can be determined arbitrarily, but depending on practical use. The typical range is 0.001 to 1 gram per 1 gram of the alkaline component of the 1-acid alkaline solution. This liquid is transparent and can be stored stably.
上記の硬化剤に適用できる珪酸アルカリは、特に限定は
なく、例えば、珪酸カリウム、Ｊｌ酸ナトリウム、珪酸
リチウム等から選ばれた１種以上が挙げられ、特に、珪
酸カリウムが好ましい。The alkali silicate that can be used as the curing agent is not particularly limited, and examples thereof include one or more selected from potassium silicate, sodium chloride, lithium silicate, etc., and potassium silicate is particularly preferred.
次に、上記の硬化剤と珪酸アルカリよりなるものは無Ｒ
繊Ｉ１１質の処理剤として使用づることか出来る。Next, the one consisting of the above curing agent and alkali silicate is R-free.
It can be used as a treatment agent for fibers.
この場合、珪酸アルカリは水溶液で仝吊に対して固形ｆ
ｆ１０〜５０％で使用するのが好ましい。その理由は、
１０％未満では固化せず、５０％を超えると取扱い上作
業性が悪いばかりでなく、硬化時間が早寸ぎ不適当であ
るからである。In this case, the alkali silicate is an aqueous solution with a solid f
It is preferable to use f10 to 50%. The reason is,
If it is less than 10%, it will not solidify, and if it exceeds 50%, it will not only be difficult to handle, but also the curing time will be too quick and inappropriate.
又、硬化剤及び珪酸アルカリの他に必要に応じて、界面
活性剤、Ｈ１泡剤、湿潤剤、水溶性有機ポリマー、水分
散性有機樹脂エマルジョン、撥水剤、着色剤、無機フィ
ラー等を添加したものも使用することができる。In addition to the curing agent and alkali silicate, surfactants, H1 foaming agents, wetting agents, water-soluble organic polymers, water-dispersible organic resin emulsions, water repellents, colorants, inorganic fillers, etc. are added as necessary. can also be used.
有ｆｉ物を添加する場合には、被処即無Ｒ線維賀のΦ量
を含めた処理後の全固形分重巾以十に対して有機物量が
１％以下とするのが好ましい。In the case of adding organic matter, it is preferable that the amount of organic matter is 1% or less based on the total solid content after treatment, including the amount of Φ of the R-free fibers to be treated.
この重量以上では耐火テスト時のｌｅ沖吊が大きくなり
好ましくない。界面活性剤としては市販のアニ外ン、ノ
ニオン、カヂオン性界面活性剤のいずれも使用できるか
、ボリイキシ１チレンアルキルフＩニル］−−チルやア
ルファオレフィンスルボンｕｔｈリウム塩が浸透性の向
上に好ましい。又、水分散性の有機樹脂１マルジ１）と
してはビニル−アクリル系具申合体エマルジョン、アク
リルスチレン共重合体エマルジョンなど使用できるが、
例えばモビニールＤＭ−７６５（ヘキス］・合成（株）
製）、ヨドゾールＡＤ−３１（カネボウＮ５Ｉ）などが
混合使用し易く、粉化防止効果を有する。If the weight exceeds this value, the le off-shore suspension during the fire resistance test will become large, which is undesirable. As a surfactant, commercially available anionic, nonionic, or cationic surfactants can be used, or polyoxy1-tyrenealkylphinyl]--thyl or alpha-olefin sulfonuthrium salts can improve permeability. preferable. In addition, as the water-dispersible organic resin 1), vinyl-acrylic composite emulsion, acrylic styrene copolymer emulsion, etc. can be used.
For example, Movinyl DM-765 (Hex) / Synthetic Co., Ltd.
), Yodozol AD-31 (Kanebo N5I), etc. are easy to mix and use and have a powdering prevention effect.
本５Ｂ明に係わる無機繊維質としては、例えば、代表的
なものどしてアスベスト、［］ツクウール、ガラスウー
ル等が挙げられるが、これらに限定されるものではない
。Typical inorganic fibers related to this 5B feature include, but are not limited to, asbestos, wool, and glass wool.
本発明の無機ａ維質の処理剤は、無機質接哲剤として主
として用いられるが、基材表何の難燃化、表面硬化等の
処理剤どして用いられる。The inorganic a-fiber treatment agent of the present invention is mainly used as an inorganic grafting agent, but it can also be used as a treatment agent for flame retardation, surface hardening, etc. of substrate surfaces.
又、その使用方法とじては、特に、無機繊維質と共に混
合する方法、無機ＩＪｉ維賀を含有する成形体に処理剤
を吹きつける方法等が挙げられるが、特に限定はない。Further, the method of using it includes, in particular, a method of mixing it with inorganic fibers, a method of spraying a treatment agent onto a molded article containing inorganic IJi Iga, etc., but there is no particular limitation.
このように、吹き付（ブ方法が採用でさることは、本光
明に係る処理剤が可使用時間が長いことの特徴によるも
のである。The reason why the spraying method is so advantageous is that the treatment agent according to the present invention has a long pot life.
アスベストの発癌性の問題がクローズアップされて以来
、近時、その各種成型品の処理、特に、建材の処理に際
してアスベスト短繊維の発塵が問題とされる。該成型品
の処理に際し、本発明に係る処理剤を用いるとその表面
から内部深くまで短繊維間を接着固化できるので発塵性
の問題がなくなり安全に処理できる。Since the carcinogenicity of asbestos has been in the spotlight, the generation of dust from short asbestos fibers has recently become a problem in the treatment of various molded products, particularly in the treatment of building materials. When processing the molded product, using the processing agent of the present invention can bond and solidify the short fibers from the surface to deep inside the product, eliminating the problem of dust generation and allowing safe processing.
以下に実施例を挙げて具体的に説明する。This will be specifically explained below with reference to Examples.
〈実施例〉
ＩＩＭアルカリ水溶液（Ａ液）の調製；ｓｉｏ ＝２
６．５％、Ｋ２０＝１３．５％の珪酸カリウム水溶ｉｆ
（以下ｒＡＫＪ ）８０重量部に水２０重量部を加えて
充分混合して、Ａ液を得た。<Example> Preparation of IIM alkaline aqueous solution (liquid A); sio = 2
6.5%, K20=13.5% potassium silicate water soluble if
20 parts by weight of water was added to 80 parts by weight of rAKJ (hereinafter referred to as rAKJ) and thoroughly mixed to obtain liquid A.
珪酸アルカリ用硬化剤（Ｂｉｔ）の調製：クエン酸４．
８３重量部を水５重量部に溶解し、これにＡＪ Ｏ＝
１６％、Ｎａ２０＝１９％のアルミン酸ソーダ水溶液１
０．１５重量部を加え、充分混合した後、更にクエン酸
７重示部を加え溶解し、次いで、アルミン酸ソーダ水溶
液を５．４５重量部を加えてｐＨ７−９とした。この混
合液５重量部に水８５重量部を加えて混合し、次いで、
グリオキザール４０％水溶故１０中Φ部を加えてＢ液を
調製した。Preparation of curing agent for alkali silicate (Bit): Citric acid 4.
83 parts by weight was dissolved in 5 parts by weight of water, and AJ O=
16%, Na20 = 19% sodium aluminate aqueous solution 1
After adding 0.15 parts by weight and thoroughly mixing, 7 parts by weight of citric acid was further added and dissolved, and then 5.45 parts by weight of an aqueous sodium aluminate solution was added to adjust the pH to 7-9. Add and mix 85 parts by weight of water to 5 parts by weight of this liquid mixture, and then
Since glyoxal was 40% aqueous, Φ part of 10 was added to prepare solution B.
硬化体の作成；Ｂ液５０ΦΦ部にＡ液５０ｆｆ！争部を
加えて良く混合し、放置して流動性のなくなるまでの時
間（硬化時間）を測定したところ６０分であった。硬化
前の同じ液を５Ｑｌ／ｌｘ １０ （１／ｎ Ｈの型枠
に流し込み硬化させた後密閉養生して１日後に圧縮強度
を測定したところ０．６に９／ｃＩ！であった（これを
「ホモゲルの圧縮強度」と表わす）、尚、測定にはアー
ムス、ラー型強度試験機を用い１Ｑ Ｉｌｌ／ｌ１ｌｉ
ｎて圧縮した。Preparation of cured body: 50ff of A liquid in 50ΦΦ part of B liquid! The mixture was added and mixed well, and the time until the mixture lost fluidity (curing time) after being left to stand was measured, and it was 60 minutes. The same liquid before hardening was poured into a mold of 5Ql/lx 10 (1/nH), cured in a sealed container, and the compressive strength was measured one day later. It was 0.6 to 9/cI! (This is expressed as "compressive strength of homogel"), and the measurement was carried out using an Arms-Lar type strength tester (1Q Ill/l1li).
It was compressed.
アスベストの処理；
アスベスト４２重量％、ポルトランドセメント２５Φ争
％、４％酢酢酸ビニルエマルミン液３３％の配合比で、
スレート板にアスベストを吹き付けた後７日放置、乾燥
して、高密度０゜２ｇ／Ｃ１３、岸さ１５ｎｎ＋の施工
品を作成し、これを１００ｍ×１０ｃＩＩに切断してテ
スト材としノζ。Asbestos treatment: 42% by weight of asbestos, 25% of Portland cement, 33% of 4% acetic acid vinyl acetate emulsion solution,
After spraying asbestos on a slate board, it was left to dry for 7 days to create a construction product with a high density of 0°2g/C13 and a bank height of 15nn+, which was then cut into 100m x 10cII pieces as test materials.
上記Ａ、８等量混合液を作成し、エアレンスガンにて４
Ｋｙ／ｒｒｌとなる第をテスト材に吹き（１け、２日欣
＠乾燥した後、アスベスト面に１０ｃｍＸ１０ｃｔｎの
塩化ビニル製支持板をエポキシ系接肴剤で全面接肴し、
アームスラー型強度試験機を用いて引張り強度試験を行
なった結束を第１表に示す。Make a mixture of 8 equal amounts of the above A, and use an air gun to
After drying, a 10 cm x 10 ctn vinyl chloride support plate was applied to the asbestos surface with an epoxy adhesive.
Table 1 shows the bundles tested for tensile strength using an Armsler type strength testing machine.
実施例２〜５及び比較例１〜５
実施例１と同様のアスベス１−処理試験をＡ液およびＢ
液の組成を変えて行なった結束を第１表に示づ。尚、表
中、ＡＮＩはＳ ｉ ０２＝２９．５％、Ｎａ２０＝
９．！＋％の珪ＦｉソーＩ／’水ｍ’ｍ、ＡＮ２はＳｉ
Ｏ＝３０．０％、Ｎａ２Ｑ＝１４．４％のＪ１酸ソータ
水溶液を表わター。Examples 2 to 5 and Comparative Examples 1 to 5 The same asbestos 1 treatment test as in Example 1 was carried out using liquids A and B.
Table 1 shows the binding performed with different liquid compositions. In addition, in the table, ANI is S i 02 = 29.5%, Na20 =
9. ! +% silicon Fi saw I/'water m'm, AN2 is Si
Represents a J1 acid sorter aqueous solution with O=30.0% and Na2Q=14.4%.
く発明の効果〉
本発明の珪酸アルカリ用硬化剤は珪酸アルカリの勧化反
応を１時間〜数時間という比較的長い硬化時間（ポット
ライフ）を有し、月つ高強度の硬化体を得ることができ
ると言う利点がある。従って、該硬化剤を用いた珪酸ア
ルカリを主成分と１６無機４ｉｉ維賀処理剤は、例えば
、アスベスト成型品９８Ｍ！の様に処即液のアスベスト
への浸透が充分になされた後に硬化するので、その内部
まで、接肴効宋が発揮できると共に、処理作衆を伴う可
使時間の許容範囲が拡大し、極めて有効である。Effects of the Invention The curing agent for alkali silicate of the present invention has a relatively long curing time (pot life) of 1 to several hours for the alkali silicate promotion reaction, and can obtain a cured product with high strength in months. It has the advantage of being able to Therefore, the 16 inorganic 4ii Iga treatment agent containing alkali silicate as the main component using this hardening agent is, for example, asbestos molded product 98M! As the treatment liquid hardens after sufficiently permeating the asbestos, it is possible to exert its adhesive effect even to the inside of the asbestos, and the permissible range of pot life with treatment is expanded, making it extremely durable. It is valid.
Claims (6)
ト及び多価アルコール酢酸エステルから選ばれた１種以
上、及びオキシカルボン酸アルミニウム錯体を含有して
なる珪酸アルカリ用硬化剤(1) A curing agent for alkali silicate containing one or more selected from aldehydes, water-soluble lower alkylene carbonates, and polyhydric alcohol acetates, and an aluminum oxycarboxylate complex.
ルである珪酸アルカリ用硬化剤(2) A curing agent for alkali silicate, wherein the aldehyde according to claim (1) is glyoxal.
ネートがエチレンカーボネートである珪酸アルカリ用硬
化剤(3) A curing agent for alkali silicate, wherein the water-soluble lower alkylene carbonate according to claim (1) is ethylene carbonate.
が多価アルコール酢酸エステルとしては、エチレングリ
コール酢酸エステル、グリセリン酢酸エステル、ソルビ
トール酢酸エステル、エチレングリコールジアセテート
から選ばれた１種以上である珪酸アルカリ用硬化剤(4) The polyhydric alcohol acetate according to claim (1) is one or more selected from ethylene glycol acetate, glycerin acetate, sorbitol acetate, and ethylene glycol diacetate. Hardening agent for alkali silicate
ム錯体がオキシカルボン酸とアルミン酸アルカリ水溶液
との反応生成物である珪酸アルカリ用硬化剤(5) A curing agent for alkali silicate, wherein the aluminum oxycarboxylate complex according to claim (1) is a reaction product of an oxycarboxylic acid and an aqueous alkali aluminate solution.
）記載の珪酸アルカリ用硬化剤及び珪酸アルカリを主成
分とする無機繊維質処理剤(6) Claims (1), (2), (3), (4) or (5)
) Hardening agent for alkali silicate and inorganic fiber treatment agent containing alkali silicate as a main component
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1070694A JP2696245B2 (en) | 1989-03-24 | 1989-03-24 | Alkali silicate curing agent, inorganic fiber treating agent containing it |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1070694A JP2696245B2 (en) | 1989-03-24 | 1989-03-24 | Alkali silicate curing agent, inorganic fiber treating agent containing it |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02252642A true JPH02252642A (en) | 1990-10-11 |
| JP2696245B2 JP2696245B2 (en) | 1998-01-14 |
Family
ID=13438997
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1070694A Expired - Fee Related JP2696245B2 (en) | 1989-03-24 | 1989-03-24 | Alkali silicate curing agent, inorganic fiber treating agent containing it |
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| Country | Link |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0798300A1 (en) * | 1996-03-09 | 1997-10-01 | Giulini Chemie GmbH | Aluminium compounds |
| WO2000014026A3 (en) * | 1998-09-02 | 2000-06-02 | Fosroc International Ltd | Water-free hardener composition |
| JP2007162351A (en) * | 2005-12-14 | 2007-06-28 | Kikusui Chemical Industries Co Ltd | Finishing method |
| JP2008534729A (en) * | 2005-04-01 | 2008-08-28 | ケイパー ホールディング エス．アール．エル | Methods and compositions for producing items |
| CN104478365A (en) * | 2014-12-25 | 2015-04-01 | 苏州中材非金属矿工业设计研究院有限公司 | Method for improving hard water resistance of magnesium aluminum silicateinorganic gel |
-
1989
- 1989-03-24 JP JP1070694A patent/JP2696245B2/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0798300A1 (en) * | 1996-03-09 | 1997-10-01 | Giulini Chemie GmbH | Aluminium compounds |
| WO2000014026A3 (en) * | 1998-09-02 | 2000-06-02 | Fosroc International Ltd | Water-free hardener composition |
| US6506246B1 (en) | 1998-09-02 | 2003-01-14 | Fosroc International Limited | Settable composition |
| JP2008534729A (en) * | 2005-04-01 | 2008-08-28 | ケイパー ホールディング エス．アール．エル | Methods and compositions for producing items |
| JP2007162351A (en) * | 2005-12-14 | 2007-06-28 | Kikusui Chemical Industries Co Ltd | Finishing method |
| CN104478365A (en) * | 2014-12-25 | 2015-04-01 | 苏州中材非金属矿工业设计研究院有限公司 | Method for improving hard water resistance of magnesium aluminum silicateinorganic gel |
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| Publication number | Publication date |
|---|---|
| JP2696245B2 (en) | 1998-01-14 |
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