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
Application number
JP6257084A
Other languages
Japanese (ja)
Other versions
JPS60204697A (en
Inventor
Takao Kitamura
Shunsaku Kato
Hideo Wada
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Agency of Industrial Science and Technology filed Critical Agency of Industrial Science and Technology
Priority to JP6257084A priority Critical patent/JPS60204697A/en
Publication of JPS60204697A publication Critical patent/JPS60204697A/en
Publication of JPH0128000B2 publication Critical patent/JPH0128000B2/ja
Granted legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides
    • C30B29/22Complex oxides
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-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
    • C30B9/00Single-crystal growth from melt solutions using molten solvents

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  • 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.,,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.

【図面の簡単な説明】[Brief explanation of drawings]

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)

【特許請求の範囲】 1 化学式Mg2B2O5で表される組成をもつホウ
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 .
JP6257084A 1984-03-29 1984-03-29 Whisker of magnesium borate and its preparation Granted JPS60204697A (en)

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)

* Cited by examiner, † Cited by third party
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

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