JPH0128000B2 - - Google Patents
Info
- Publication number
- JPH0128000B2 JPH0128000B2 JP6257084A JP6257084A JPH0128000B2 JP H0128000 B2 JPH0128000 B2 JP H0128000B2 JP 6257084 A JP6257084 A JP 6257084A JP 6257084 A JP6257084 A JP 6257084A JP H0128000 B2 JPH0128000 B2 JP H0128000B2
- Authority
- JP
- Japan
- Prior art keywords
- magnesium
- magnesium borate
- whiskers
- sodium
- chloride
- 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.)
- Expired
Links
- NFMWFGXCDDYTEG-UHFFFAOYSA-N trimagnesium;diborate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]B([O-])[O-].[O-]B([O-])[O-] NFMWFGXCDDYTEG-UHFFFAOYSA-N 0.000 claims description 26
- 239000011777 magnesium Substances 0.000 claims description 13
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 8
- 239000004327 boric acid Substances 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229910052749 magnesium Inorganic materials 0.000 claims description 7
- 239000000395 magnesium oxide Substances 0.000 claims description 7
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 7
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052810 boron oxide Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 4
- 239000000347 magnesium hydroxide Substances 0.000 claims description 4
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 2
- 239000000463 material Substances 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 description 5
- 235000010755 mineral Nutrition 0.000 description 5
- 239000011707 mineral Substances 0.000 description 5
- 239000003513 alkali Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000002657 fibrous material Substances 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010908 decantation Methods 0.000 description 2
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- GDTSJMKGXGJFGQ-UHFFFAOYSA-N 3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B([O-])OB2OB([O-])OB1O2 GDTSJMKGXGJFGQ-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910019440 Mg(OH) Inorganic materials 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 magnesium borate compound Chemical class 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B9/00—Single-crystal growth from melt solutions using molten solvents
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明は新規なホウ酸マグネシウムウイスカー
及びその製造方法に関し、さらに詳しくいえば、
耐アルカリ性、耐熱性、中性子吸収能、絶縁性、
光輝性及び光透過性などの性質を有し、ろ材、ラ
イニング材、断熱材、中性子吸収材、難燃材及び
隔膜などの素材として有用なホウ酸マグネシウム
ウイスカー及びその製造方法に関するものであ
る。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a novel magnesium borate whisker and a method for producing the same.
Alkali resistance, heat resistance, neutron absorption ability, insulation,
The present invention relates to magnesium borate whiskers, which have properties such as brightness and light transmittance and are useful as materials for filter media, lining materials, heat insulating materials, neutron absorbers, flame retardants, diaphragms, etc., and a method for producing the same.
従来、化学式Mg2B2O5で表わされるホウ酸マ
グネシウムはマグネシウムパイロボレートと総称
され、スアナイトの名称をもつ単斜晶系の鉱物と
人工合成による三斜晶系の鉱物が知られている。
前者のスアナイトは北朝鮮のスアン地区で標本程
度の量が見出されている塊状鉱物であつて、その
組織の一部として繊維状物を含むが、繊維状物と
しては単離されず、常にケイ素、アルミニウム、
鉄、銅などの不純物と共存した形の塊状物として
得られている。 Conventionally, magnesium borate represented by the chemical formula Mg 2 B 2 O 5 is collectively called magnesium pyroborate, and a monoclinic mineral called suanite and an artificially synthesized triclinic mineral are known.
The former, suanite, is a massive mineral found in specimen-sized quantities in the Suan area of North Korea, and although it contains fibrous materials as part of its structure, it is not isolated as fibrous materials and always contains silicon. ,aluminum,
It is obtained as a lump that coexists with impurities such as iron and copper.
他方、ホウ酸マグネシウムの合成については、
例えばホウ酸とマグネシウム塩との混合物から天
然産のものと同じＸ線回折図形をもつスアナイト
の合成が報告されている〔W.Berdesinski；
Neues Jahrb.Mineral.Monatsh.，５，106〜111
（1955）〕。しかしながら、このものは粉末状であ
り、繊維状又はウイスカー状のものは得られてい
ない。また人工合成による三斜晶系の合成
Mg2B2O5については、平板状又は短いプリズム
状の結晶のものが知られているが、ウイスカーは
これまで知られていない。 On the other hand, regarding the synthesis of magnesium borate,
For example, the synthesis of suanite with the same X-ray diffraction pattern as naturally occurring suanite from a mixture of boric acid and magnesium salt has been reported [W. Berdesinski;
Neues Jahrb. Mineral. Monatsh., 5 , 106-111
(1955)]. However, this product is in powder form, and fibrous or whisker-like products have not been obtained. Synthesis of triclinic system by artificial synthesis
As for Mg 2 B 2 O 5 , flat or short prismatic crystals are known, but whiskers have not been known so far.
本発明者らは、このような事情に鑑み、ライニ
ング材や断熱材などの素材として有用な、ホウ酸
マグネシウム化合物から成るウイスカーを開発す
るために鋭意研究を重ねた結果、溶融剤としてナ
トリウム又はカリウムの塩化物を用い、所定のマ
グネシウム供給成分とホウ酸供給成分とを所定の
温度で反応させることにより、その目的を達成し
うることを見出し、この知見に基づいて本発明を
完成するに至つた。 In view of these circumstances, the inventors of the present invention have conducted extensive research to develop whiskers made of magnesium borate compounds that are useful as materials for lining materials, insulation materials, etc. The inventors have discovered that the objective can be achieved by reacting a specified magnesium supplying component and a boric acid supplying component at a specified temperature using a chloride, and based on this knowledge, they have completed the present invention. .
すなわち、本発明は、化学式Mg2B2O5で表わ
される新規なホウ酸マグネシウムウイスカー及び
その製造方法を提供するものである。このホウ酸
マグネシウムウイスカーは、ASTM粉末Ｘ線回
折カード16−168のスアナイトと類似したＸ線回
折図形を与えるが、〔201〕面及び〔402〕面が発
達している点で特異的であり、このようなホウ酸
マグネシウム化合物のウイスカーは文献未載の新
規な物質である。 That is, the present invention provides a novel magnesium borate whisker represented by the chemical formula Mg 2 B 2 O 5 and a method for producing the same. This magnesium borate whisker gives an X-ray diffraction pattern similar to that of suanite in ASTM powder X-ray diffraction card 16-168, but is unique in that [201] and [402] planes are developed. Such a whisker of a magnesium borate compound is a novel substance that has not been described in any literature.
このホウ酸マグネシウムウイスカーは、例えば
酸化マグネシウム、水酸化マグネシウム及び塩化
マグネシウムの中から選ばれたマグネシウム供給
成分と、酸化ホウ素及びホウ酸ナトリウムの中か
ら選ばれたホウ酸供給成分とを塩化ナトリウム及
び塩化カリウムの中から選ばれた少なくとも１種
の溶融剤の存在下、600〜1000℃の温度に加熱し
て反応させることによつて製造することができ
る。 This magnesium borate whisker combines, for example, a magnesium supply component selected from magnesium oxide, magnesium hydroxide, and magnesium chloride, and a boric acid supply component selected from boron oxide and sodium borate. It can be produced by heating and reacting at a temperature of 600 to 1000° C. in the presence of at least one melting agent selected from potassium.
この方法におけるマグネシウム供給成分として
は、酸化マグネシウム、水酸化マグネシウム及び
塩化マグネシウムが用いられる。これらは単独で
用いてもよいし、また２種以上混合して用いても
よい。 Magnesium oxide, magnesium hydroxide and magnesium chloride are used as magnesium supply components in this method. These may be used alone or in combination of two or more.
次にホウ酸供給成分としては、酸化ホウ素や各
種ホウ酸のナトリウム塩、例えばオルトホウ酸ナ
トリウム（Na3BO3）、四ホウ酸ナトリウム
（Na2B4O7）、メタホウ酸ナトリウム（NaBO3）
などが用いられる。これらは単独で用いてもよい
し、また２種以上混合して用いてもよい。 Next, boric acid supply components include boron oxide and various sodium salts of boric acid, such as sodium orthoborate (Na 3 BO 3 ), sodium tetraborate (Na 2 B 4 O 7 ), and sodium metaborate (NaBO 3 ).
etc. are used. These may be used alone or in combination of two or more.
本発明方法に従えば、前記のマグネシウム供給
成分とホウ酸供給成分とをマグネシウムとホウ素
のモル比１：４から１：１の範囲の割合で混合
し、さらに溶融剤を全重量に基づき10〜95重量％
の範囲で添加し、600〜1000℃の範囲の温度に加
熱して反応させることによつて所望のホウ酸マグ
ネシウムウイスカーを生成させることができる。
この際の加熱温度が600℃未満では、反応の進行
が極めて遅いし、また1000℃を超えると目的とす
るホウ酸マグネシウムウイスカーの外に三斜晶系
のプリズム状ホウ酸マグネシウムが多量に副生す
るので好ましくない。反応時間は、通常15分から
２時間の範囲である。 According to the method of the present invention, the above-mentioned magnesium supply component and boric acid supply component are mixed in a molar ratio of magnesium to boron ranging from 1:4 to 1:1, and a melting agent is further added to 95% by weight
Desired magnesium borate whiskers can be produced by adding in a range of 1,000 °C and heating to a temperature in a range of 600 to 1,000°C to cause a reaction.
If the heating temperature is less than 600℃, the reaction progresses extremely slowly, and if it exceeds 1000℃, a large amount of triclinic prismatic magnesium borate will be produced as a by-product in addition to the desired magnesium borate whiskers. Therefore, it is not desirable. The reaction time usually ranges from 15 minutes to 2 hours.
この反応生成物からウイスカーを単離するに
は、先ず熱水あるいは冷水で処理して溶融剤その
他の水溶性成分を除去する。用いた原料組成によ
り副生物がある場合には、残留物からデカンテー
シヨン、水ひ、気泡分離などの手段で繊維状物を
分離する。次いでこのようにして得られた粗製ホ
ウ酸マグネシウムウイスカーをアルカリ例えば水
酸化ナトリウム水溶液及び酸例えば酢酸水溶液あ
るいは冷希塩酸を用いて洗浄し、不純物を除去す
れば純粋なホウ酸マグネシウムウイスカーが得ら
れる。 To isolate whiskers from this reaction product, the whiskers are first treated with hot or cold water to remove the melting agent and other water-soluble components. If by-products are present due to the composition of the raw materials used, the fibrous materials are separated from the residue by means such as decantation, hydration, and bubble separation. The crude magnesium borate whiskers thus obtained are then washed with an alkali such as an aqueous sodium hydroxide solution and an acid such as an acetic acid aqueous solution or cold dilute hydrochloric acid to remove impurities, yielding pure magnesium borate whiskers.
このようにして得られたホウ酸マグネシウムウ
イスカーは、そのＸ線回折スペクトルにおいて、
ASTM粉末Ｘ線回折カード16−168に比べｄ値
4.47の〔201〕面及びｄ値2.823の〔402〕面の回
折強度が強く、ｄ値2.557の〔012〕面の回折強度
が相対的に弱くなつており、したがつて、このも
のは繊維状化合物であると同定することができ
る。 In the X-ray diffraction spectrum of the magnesium borate whiskers obtained in this way,
d value compared to ASTM powder X-ray diffraction card 16-168
The diffraction intensity of the [201] plane of 4.47 and the [402] plane of d value 2.823 is strong, and the diffraction intensity of the [012] plane of d value 2.557 is relatively weak. Therefore, this material is fibrous. It can be identified as a compound.
前記のようにして、単離されたホウ酸マグネシ
ウムウイスカーは、長さ0.01〜５mm、太さ１〜
100μm、アスペクト比10〜200の無色透明の長針
状結晶であつて、常温の鉱酸にはかなりの耐性を
有し、例えば3M−塩酸中に３日間浸漬しても見
掛け上大きな変化を示さず、また濃熱アルカリに
も容易には侵されない。さらに、このものは明確
な融点を約1300℃にもつている点においても文献
〔Mary E.Mrosc and Michael Fleischer；
American Mineralogist，48，915〜924（1963）〕
記載の化合物とは異なる。 The magnesium borate whiskers isolated as described above have a length of 0.01 to 5 mm and a thickness of 1 to 5 mm.
It is a colorless and transparent long acicular crystal with a diameter of 100μm and an aspect ratio of 10 to 200, and has considerable resistance to mineral acids at room temperature.For example, it does not show any significant change in appearance even when immersed in 3M hydrochloric acid for 3 days. , and is not easily attacked by concentrated alkali. Furthermore, this material has a definite melting point of about 1300℃, as described in the literature [Mary E. Mrosc and Michael Fleischer;
American Mineralogist, 48 , 915-924 (1963)]
Different from the described compound.
本発明のホウ酸マグネシウムウイスカーは、耐
アルカリ性、耐熱性、中性子吸収能、絶縁性、光
輝性及び光透過性などの性質を有し、ろ材、ライ
ニング材、断熱材、中性子吸収材、難燃材及び隔
膜などの素材として極めて有用である。 The magnesium borate whiskers of the present invention have properties such as alkali resistance, heat resistance, neutron absorption ability, insulation, brightness, and light transparency, and can be used as filter media, lining materials, heat insulation materials, neutron absorption materials, and flame retardant materials. It is also extremely useful as a material for diaphragms, etc.
次に実施例によつてこの発明をさらに詳細に説
明する。 Next, the present invention will be explained in more detail with reference to Examples.
実施例 １
酸化マグネシウム（MgO）４ｇと酸化ホウ素
（B2O3）７ｇ及び溶融剤として塩化ナトリウム27
ｇを、アルミナ製るつぼに採取し、電気炉中850
℃で５時間反応させる。反応物を徐冷したのち、
１の蒸留水で煮沸する。煮沸によつて溶融剤を
除去した残留物を水洗することにより、粗製ホウ
酸マグネシウムを得る。続いてデカンテーシヨン
により微量の非繊維状副生物を分離し、ホウ酸マ
グネシウムウイスカー7.0ｇを得る。こうして得
たウイスカーは、1300℃に融点を持ち、元素分析
値（Mg2B2O5として）は
Mg Ｂ Ｏ
計算値（％） 32.4 14.4 53.2
実測値（％） 31.9 14.1 54.0
であつた。Example 1 4 g of magnesium oxide (MgO), 7 g of boron oxide (B 2 O 3 ) and 27 g of sodium chloride as a melting agent
850 g was collected in an alumina crucible and heated in an electric furnace at 850 g.
React at ℃ for 5 hours. After slowly cooling the reactant,
Boil with distilled water. Crude magnesium borate is obtained by washing the residue from which the melting agent has been removed by boiling with water. Subsequently, trace amounts of non-fibrous by-products are separated by decantation to obtain 7.0 g of magnesium borate whiskers. The whiskers thus obtained had a melting point of 1300° C., and the elemental analysis values (as Mg 2 B 2 O 5 ) were as follows: Mg B O Calculated value (%) 14.4 53.2 Actual value (%) 31.9 14.1 54.0.
この方法で得られたホウ酸マグネシウムウイス
カーのＸ線回折図形を第１図に、２次電子線像を
第２図に示す。 The X-ray diffraction pattern of the magnesium borate whiskers obtained by this method is shown in FIG. 1, and the secondary electron beam image is shown in FIG.
実施例 ２
実施例１における酸化マグネシウムと酸化ホウ
素の代りに、塩化マグネシウム（MgCl2）10.4ｇ
及び四ホウ酸ナトリウム（Na2B4O7）21.2ｇを、
また溶融剤としては塩化ナトリウムと塩化カリウ
ムの等モル混合物27ｇを用いて、750℃で３時間
反応させる。反応後、炉内で自然冷却したのち、
分離は実施例１と同じ方法で行い、ホウ酸マグネ
シウムウイスカー繊維4.2ｇを得た。さらに、水
ひに続いて100℃の1M水酸化ナトリウム溶液及び
１規定の冷塩酸で不純物を溶解し去ることによ
り、純粋なホウ酸マグネシウムウイスカー2.0ｇ
を得た。Example 2 10.4 g of magnesium chloride (MgCl 2 ) was used instead of magnesium oxide and boron oxide in Example 1.
and 21.2 g of sodium tetraborate (Na 2 B 4 O 7 ),
Further, as a melting agent, 27 g of an equimolar mixture of sodium chloride and potassium chloride was used, and the reaction was carried out at 750° C. for 3 hours. After the reaction, after cooling naturally in the furnace,
Separation was performed in the same manner as in Example 1 to obtain 4.2 g of magnesium borate whisker fibers. Furthermore, 2.0 g of pure magnesium borate whiskers were obtained by dissolving impurities with 1M sodium hydroxide solution at 100°C and 1N cold hydrochloric acid.
I got it.
実施例 ３
実施例１における酸化マグネシウムと酸化ホウ
素の代りに水酸化マグネシウム（Mg（OH）2）5.8
ｇ及びメタホウ酸ナトリウム（NaBO2・4H2O）
21.0ｇを用い、300℃まで徐々に加熱したのち、
温度800℃で15時間反応させる。分離は実施例１
と同様に行つてホウ酸マグネシウムウイスカー繊
維3.7ｇを得た。Example 3 Magnesium hydroxide (Mg(OH) 2 )5.8 was used instead of magnesium oxide and boron oxide in Example 1.
g and sodium metaborate (NaBO 2 4H 2 O)
After gradually heating to 300℃ using 21.0g,
React at a temperature of 800℃ for 15 hours. Separation is Example 1
In the same manner as above, 3.7 g of magnesium borate whisker fibers were obtained.
第１図は、本発明のホウ酸マグネシウムウイス
カーの１例のＸ線回折図である。第２図は、本発
明のホウ酸マグネシウムウイスカーの１例の繊維
の形状を示す写真である。
FIG. 1 is an X-ray diffraction diagram of an example of magnesium borate whiskers of the present invention. FIG. 2 is a photograph showing the shape of fibers of an example of the magnesium borate whisker of the present invention.
Claims (1)
酸マグネシウムウイスカー。 ２ 酸化マグネシウム、水酸化マグネシウム及び
塩化マグネシウムの中から選ばれたマグネシウム
供給成分と、酸化ホウ素及びホウ酸ナトリウムの
中から選ばれたホウ酸供給成分とを、塩化ナトリ
ウム及び塩化カリウムの中から選ばれた少なくと
も１種の溶融剤の存在下、600〜1000℃の温度に
加熱して反応させることを特徴とする、化学式
Mg2B2O5で表わされる組成をもつホウ酸マグネ
シウムウイスカーの製造方法。[Claims] 1. Magnesium borate whiskers having a composition represented by the chemical formula Mg 2 B 2 O 5 . 2. A magnesium supplying component selected from magnesium oxide, magnesium hydroxide, and magnesium chloride, and a boric acid supplying component selected from boron oxide and sodium borate, and a boric acid supplying component selected from sodium chloride and potassium chloride. The chemical formula is characterized in that the reaction is carried out by heating to a temperature of 600 to 1000 °C in the presence of at least one melting agent.
A method for producing magnesium borate whiskers having a composition represented by Mg 2 B 2 O 5 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6257084A JPS60204697A (en) | 1984-03-29 | 1984-03-29 | Whisker of magnesium borate and its preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6257084A JPS60204697A (en) | 1984-03-29 | 1984-03-29 | Whisker of magnesium borate and its preparation |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60204697A JPS60204697A (en) | 1985-10-16 |
| JPH0128000B2 true JPH0128000B2 (en) | 1989-05-31 |
Family
ID=13204084
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6257084A Granted JPS60204697A (en) | 1984-03-29 | 1984-03-29 | Whisker of magnesium borate and its preparation |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60204697A (en) |
Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63319299A (en) * | 1987-06-20 | 1988-12-27 | Agency Of Ind Science & Technol | Aluminum borate whisker and production thereof |
| JPS63319298A (en) * | 1987-06-20 | 1988-12-27 | Agency Of Ind Science & Technol | Aluminum borate whisker and production thereof |
| WO1996014359A1 (en) * | 1994-11-04 | 1996-05-17 | Daikin Industries, Ltd. | Molten fluororesin composition |
| JP3007548B2 (en) * | 1995-01-27 | 2000-02-07 | 日光化成株式会社 | Insulated electrical insulator composition |
| CN100375795C (en) * | 2006-09-08 | 2008-03-19 | 清华大学 | Magnesium borate whisker hydrothermal synthesis preparation method |
| CN102633274A (en) * | 2011-02-15 | 2012-08-15 | 长春理工大学 | Two-step preparation method of Mg2B2O5 one-dimensional nanorod |
| CN103008652B (en) * | 2012-12-12 | 2014-08-13 | 成都理工大学 | Method for preparing magnesium oxide whisker/ magnesium composite powder by in-situ growth on surface of magnesium powder |
| CN109292790B (en) * | 2018-12-19 | 2022-02-15 | 中国科学院青海盐湖研究所 | Preparation method of basic magnesium borate nanorod |
| CN112144120B (en) * | 2020-10-15 | 2022-06-10 | 陕西嘉裕化工有限公司 | Production process of magnesium borate whisker |
| CN112877783B (en) * | 2021-01-11 | 2022-04-01 | 东北大学 | Method for preparing magnesium borate whisker by using magnesite |
| CN112897991A (en) * | 2021-03-12 | 2021-06-04 | 武汉科技大学 | Magnesium borate whisker porous ceramic material based on molten salt growth method and preparation method thereof |
-
1984
- 1984-03-29 JP JP6257084A patent/JPS60204697A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60204697A (en) | 1985-10-16 |
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