JPS60264328A - Synthesis of bi2moo6 of koechlinite type - Google Patents
Synthesis of bi2moo6 of koechlinite typeInfo
- Publication number
- JPS60264328A JPS60264328A JP59122773A JP12277384A JPS60264328A JP S60264328 A JPS60264328 A JP S60264328A JP 59122773 A JP59122773 A JP 59122773A JP 12277384 A JP12277384 A JP 12277384A JP S60264328 A JPS60264328 A JP S60264328A
- Authority
- JP
- Japan
- Prior art keywords
- type
- bi2moo6
- coniclinite
- gamma
- koechlinite
- 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
- 230000015572 biosynthetic process Effects 0.000 title description 3
- 238000003786 synthesis reaction Methods 0.000 title description 3
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 15
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 10
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 abstract description 18
- 230000007704 transition Effects 0.000 abstract description 14
- 239000000203 mixture Substances 0.000 abstract description 13
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract description 12
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 abstract description 6
- 238000010586 diagram Methods 0.000 abstract description 4
- 229910002900 Bi2MoO6 Inorganic materials 0.000 abstract 4
- 206010027476 Metastases Diseases 0.000 description 9
- 230000009401 metastasis Effects 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- QXYJCZRRLLQGCR-UHFFFAOYSA-N dioxomolybdenum Chemical compound O=[Mo]=O QXYJCZRRLLQGCR-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 238000003825 pressing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000002427 irreversible effect Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001308 synthesis method Methods 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- 229910000417 bismuth pentoxide Inorganic materials 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分骨
本発明はコニクリナイト型Ｂ１２Ｍ００６の合成法に関
する。コニクリナイト型Ｂ１２Ｍ０Ｏ６は不飽和炭化水
素の酸化触媒として有効寿ものであり、特にプロピレン
からアクリルニトリルを合成する触媒として重要外もの
である。DETAILED DESCRIPTION OF THE INVENTION Industrial Application The present invention relates to a method for the synthesis of coniclinite type B12M006. Coniclinite type B12M0O6 has a long life as an oxidation catalyst for unsaturated hydrocarbons, and is particularly unimportant as a catalyst for synthesizing acrylonitrile from propylene.
従来技術
従来のコニクリナイト型Ｂ１２Ｍ００６の合成法としく
１ ）
一国は、湿式法と乾式法が知られている。Prior Art Conventional methods for synthesizing coniclinite type B12M006: 1) A wet method and a dry method are known in one country.
湿式法では、例えば（ＮＨ４）６ＭＯ７０２４・４Ｈ２
０を溶解したアンモニア水溶液と％ Ｂｉ（Ｎｏ５）、
・５Ｈ２０を溶解した硝酸水溶液とを混合して、ｐＩ（
８の状態で約８０℃に１時間保持［７た後、濃アンモニ
ア水でｐＨＩ］とかし蒸発乾固し、これを５００℃で約
２０時間加熱することにより合成されていた。この合成
法によるときは、溶液の調整とｐＨの調整に多大の労力
と薬剤を必要とするばかシで彦＜、更に蒸発乾固・仮焼
の多工程と長時間を必要とする問題点があった。In the wet method, for example, (NH4)6MO7024.4H2
Ammonia aqueous solution in which 0 was dissolved and % Bi (No5),
・Mix with a nitric acid aqueous solution in which 5H20 is dissolved to obtain pI (
It was synthesized by holding the mixture at about 80° C. for 1 hour in the state of 8 [7, then pHI with concentrated aqueous ammonia], evaporating to dryness, and heating this at 500° C. for about 20 hours. When using this synthesis method, there are problems in that it requires a lot of labor and chemicals to prepare the solution and adjust the pH, and it also requires multiple steps of evaporation to dryness and calcination and a long time. there were.
乾式法でけ％ Ｂｉ２Ｏ３または熱分解によりＢ１２０
うを生成するＢｉ化合物と、Ｗｏｏ３ｔたは熱分解によ
りＭｏｏ、を生成するＭｏ化合物とを混合し、この混合
物を５００〜６００°Ｃで加熱することによね合成して
いた。この方法によるときは、反応可能温度の範囲が狭
く、比較的高温を必要とし、反応終結に長時間を要する
。また加熱温度を５００℃以下にすると反応性が低下し
、未反応のものが残る欠点があった。B120 by dry method % Bi2O3 or thermal decomposition
Synthesis was accomplished by mixing a Bi compound that produces a molten metal with a Mo compound that produces Woo3t or Moo by thermal decomposition, and heating this mixture at 500 to 600°C. This method has a narrow reaction temperature range, requires a relatively high temperature, and takes a long time to complete the reaction. Furthermore, when the heating temperature is lower than 500° C., the reactivity decreases and there is a drawback that unreacted substances remain.
Ｑ １
発明の目的
本発明は従来法における欠点を解消すべくなされたもの
で、その目的は、溶液及びｐＨの調整を必要とせず、少
工程、小労力で容易に、かつ短時間で、優れたコニクリ
ナイト型Ｂ１２Ｍ００６を合成する方法を提供するにあ
る。Q1 Purpose of the Invention The present invention was made to solve the drawbacks of conventional methods.The purpose is to easily and quickly produce an excellent solution without requiring adjustment of solution and pH, with few steps and little labor. The present invention provides a method for synthesizing coniclinite type B12M006.
発明の構成
りｉ２Ｍｏｂ６化合物には熱力学的に安定々同質異像の
ものとしてコニクリナイト型のほかγ′型と称するもの
がある。コニクリナイト型は斜方晶系に属し、ａ ＝
５．５０６１ 、 ｂ ＝ ５．４８７ Ｘ 、 Ｃ＝
１６．２２６叉であり、γ′型は単斜晶系に属し、ａ
＝１７．２５１ Ｘ。Structure of the Invention Among the i2Mob6 compounds, there are thermodynamically stable isomorphic compounds called the γ' type as well as the coniclinite type. The coniclinite type belongs to the orthorhombic system, and a =
5.5061, b = 5.487 X, C=
16.226 prongs, the γ' type belongs to the monoclinic system, and the a
=17.251X.
ｂ ＝ ２２．４２２ Ｘ 、 ｃ ＝ ５．８５１
Ｘ、β＝８９°３０′である。コニクリナイト型は空中
で加熱されると、６００℃附近で準安定相のγ′となり
、次いで６６０°Ｃ附近でγ′型に転位する。しかしな
がら、冷却過程、ｊ、、・ ″パ″Ｃｈｒ’９”“°”
？１Ｊ−）（）“へ°１”１見られない。即ち、γ′型
への転移は不可逆であり、γ′型が室温でも安定に存在
する。b = 22.422X, c = 5.851
X, β=89°30'. When the coniclinite type is heated in air, it becomes a metastable γ' phase at around 600°C, and then transforms to the γ' type at around 660°C. However, during the cooling process, j...
? 1J-) () "to °1" 1 not seen. That is, the transition to the γ' form is irreversible, and the γ' form exists stably even at room temperature.
しかしながら、γ′型は準安定相であるため、６００”
ニー４．１ｅ６ｏ°Ｃの温度領域においては時間の経過
と共に徐々にγ′型へ転移する。このため、６００℃以
上で熱処理すると、γ′型のＢｉ２Ｍｏｂ６となる。従
ってコニクリナイト型Ｂ１２Ｗｏｏ６を得るためには大
気圧下では６００℃より低い温度で加熱しなければなら
ない。しかし、この温度領域では反応性が低い。However, since the γ′ type is a metastable phase, the 600”
In the temperature range of 4.1e6o°C, it gradually transitions to the γ' type with the passage of time. Therefore, when heat treated at 600° C. or higher, it becomes γ'-type Bi2Mob6. Therefore, in order to obtain coniclinite type B12Woo6, it is necessary to heat at a temperature lower than 600° C. under atmospheric pressure. However, reactivity is low in this temperature range.
不発８ＡＳらは、コニクリナイト型Ｂ１２Ｍ００６の熱
力学的安定領域について鋭意研究の結果、この化合物が
高圧安定相であることを見出し、圧力を加えながら、γ
′型Ｂ１２Ｍ００６を加熱すると、これまで不可逆と考
えられていたコニクリナイト型Ｂ１２Ｍ０Ｏ６への転移
を容易に行わしめうろこと、またγ′型Ｂｉ、、Ｗｏｏ
３に代え、熱分解によってＢｉ２Ｏ３を生成するＢ１化
合物と、熱分解によりＭ２Ｏ３を生成するＭ。As a result of intensive research on the thermodynamic stability region of coniclinite type B12M006, Misfire 8AS et al. discovered that this compound is a high-pressure stable phase, and while applying pressure, γ
When '-type B12M006 is heated, it easily undergoes a transition to coniclinite-type B12M0O6, which was previously thought to be irreversible.
3, a B1 compound that generates Bi2O3 through thermal decomposition and M that generates M2O3 through thermal decomposition.
化合物の粉末を、Ｂｉ２Ｏ５： ＭｏＯ３のモル比で約
１＝１の割合で混合した混合物を圧力を加えながら加熱
すると、反応が著しく促進され、５００°Ｃ以下の温度
でもコニクリナイト型Ｂ１２Ｍ０Ｏ６を合成し得ること
を究明し得た。この知見に基いて本発明を完成した。By heating a mixture of compound powders at a molar ratio of Bi2O5: MoO3 of approximately 1=1 while applying pressure, the reaction is significantly accelerated, and coniclinite type B12M0O6 can be synthesized even at temperatures below 500°C. I was able to find out. The present invention was completed based on this knowledge.
２１６発明の要旨はγ′型Ｂ１２Ｗｏｏ６または、熱分
解により Ｂｉ２Ｏ，を生成するＢｉ化合物と熱分解に
よりＭｏＯ２を生成するＭＯ化合物の粉末をＢｉ２Ｏ３
： ＭｏＯ２のモル比で１＝１の割合で混合した混合物
を１５０に９７ｃｍ２以上に加圧しながら４００〜６０
０°Ｃに加熱することを特徴とするコニクリナイト型Ｂ
１２Ｍ００６の合成法にある。216 The gist of the invention is to combine powders of γ'-type B12Woo6 or Bi compounds that generate Bi2O through thermal decomposition and MO compounds that generate MoO2 through thermal decomposition into Bi2O3.
: A mixture of MoO2 mixed at a molar ratio of 1=1 was heated to 150 to 400 to 600 cm while pressurizing it to 97 cm2 or more.
Coniclinite type B characterized by heating to 0°C
12M006.
第１図はコニクリナイト型Ｂｉ２Ｍｏｂ６とγ′型Ｂ１
２Ｗｏｏ６についての圧力一温度相平衡図であり、領域
Ａはコニクリナイト型Ｂ１２Ｍ００６が安定に存在でき
る領域で、領域Ｂはγ′型Ｂ１２Ｍ０Ｏ６が安定に存在
できる領域を示す。第２図は本発明の方法による転移に
よυコニクリナイト型Ｂｉ２Ｍｏｂ６を生成することが
可能な温度−圧力範囲を示す。斜線で囲まれた領域Ａは
γ′型からコニクリナイト型Ｂｉ２Ｍｏｂ６への転移が
１２０時間以内に行われる領域で、線分Ｂは従来技術で
コニクリナイト型Ｂ１２Ｍ００６の合成が可能であった
領域である。点線で表わされた面線はγ′型Ｂ１゜Ｍ２
Ｏ３とコニクリナイト型Ｂ１２Ｍ００６の安定領域の境
界線を示す。Figure 1 shows coniclinite type Bi2Mob6 and γ' type B1.
This is a pressure-temperature phase equilibrium diagram for 2Woo6, where region A is a region where coniclinite type B12M006 can stably exist, and region B shows a region where γ' type B12M0O6 can stably exist. FIG. 2 shows the temperature-pressure range in which υconiclinite type Bi2Mob6 can be produced by transformation according to the method of the present invention. Region A surrounded by diagonal lines is a region where the transition from γ' type to coniclinite type Bi2Mob6 takes place within 120 hours, and line segment B is a region where coniclinite type B12M006 could be synthesized using the conventional technique. The dotted surface line is γ′ type B1°M2
The boundary between the stability regions of O3 and coniclinite type B12M006 is shown.
（５）
第１図が示すように、大気圧下でのコニクリナイト型Ｂ
１２Ｍ００６からγ′型８１２Ｍ０ｏ６ヘノ転移温度は
約５７０℃である。そして第２図における温度軸上に太
線で示す部分が従来の乾式合成法による転移温度範囲で
、本発明による転移範囲が広い面的広がりを持つことが
わかる。(5) As shown in Figure 1, coniclinite type B under atmospheric pressure
The transition temperature of 12M006 to γ' form 812M0o6 is about 570°C. The part indicated by the thick line on the temperature axis in FIG. 2 is the transition temperature range according to the conventional dry synthesis method, and it can be seen that the transition range according to the present invention has a wide area spread.
コニクリナイト型Ｂ１２Ｗｏｏ６を生成する反応の進行
は、圧力と温度と加熱時間に依存する。同一温度に加熱
した実験では圧力が高い程転移あるいは反応の完予時間
が短かくてすむ。また同一圧力に保持した実験では、温
度が高い程転移あるいは反応の完了時間は短かくなる。The progress of the reaction that produces coniclinite type B12Woo6 depends on pressure, temperature, and heating time. In an experiment where heating to the same temperature is performed, the higher the pressure, the shorter the time required to complete the transition or reaction. Also, in experiments where the pressure was maintained at the same level, the higher the temperature, the shorter the time to complete the transition or reaction.
ｒｌ型Ｂｉ２Ｍｏｂ６を出発原料として使用した場合に
おける圧力、温度及び加熱時間と転移の進行状況を示す
と次の通りであった。The pressure, temperature, heating time, and progress of transition when rl type Bi2Mob6 was used as the starting material were as follows.
（６）
第 １ 表
温１１１（’Ｃ） 圧力（Ｋ９／Ｃｍ２） 時間（ｈ）
結 果４００ １５００ ２］ 不十分
４００ １５００ ４７ 完全転移
４００ １０００ ４９ 不十分
４００ １０００ ８０ 完全転移
４００ ８００ １２０ 完全転移
４００ ６５０ １２０ 不十分
５００ １５００ １ 不十分
５００ １５００ ３ 完全転移
５００ １０００ １ 不十分
５００ １０００ ３ 完全転移
５００ ５００ ４８ 不十分
５００ ５００ ７２ 完全転移
５００ １５０ １２０ 完全転移
５５０ １５００ １ 不十分
５５０ １５００ ２ 完全転移
イｌ’ ５５０ １０００ ７ 不十分６００ １００
０ ４９ 完全転移
１ｉＪの結果が示すように、４００℃〜６００°Ｃで容
易にコニクリナイト型Ｂ１２Ｗｏｏ６が得られ、加熱の
際に必要な最小圧力は温度によって異なる。例えば、転
移が１２０時間以内に完了するためには４００°Ｃで８
００ Ｋ９／ｃｍ２．５００℃で１５０ Ｋｙ／ｃｍ２
．６００℃で１０００Ｋｙ／ｃｍ２である。(6) 1st table temperature 111 ('C) pressure (K9/Cm2) time (h)
Result 400 1500 2] Insufficient 400 1500 47 Complete metastasis 400 1000 49 Insufficient 400 1000 80 Complete metastasis 400 800 120 Complete metastasis 400 650 120 Insufficient 500 1500 1 Insufficient 500 1500 3 Complete metastasis 500 1000 1 Insufficient 500 1000 3 Complete metastasis 500 500 48 Insufficient 500 500 72 Complete metastasis 500 150 120 Complete metastasis 550 1500 1 Insufficient 550 1500 2 Complete metastasis I' 550 1000 7 Insufficient 600 100
0 49 Complete transition As shown by the results of 1 iJ, coniclinite type B12Woo6 is easily obtained at 400° C. to 600° C., and the minimum pressure required during heating varies depending on the temperature. For example, in order for the metastasis to be completed within 120 hours, at 400°C
00 K9/cm2.150 Ky/cm2 at 500℃
．． It is 1000 Ky/cm2 at 600°C.
本発明の方法ではγ’ −Ｂｉ２Ｍｏｏ、に代えて、熱
分解によりＢｉ２Ｏ３，Ｍｏｂ、を生成するＢ、を化合
物とＭｏ化合物をＢｉ２Ｏ，： ＭｏＯ５のモル比で１
：１の割合で混合物を使用しても同様にコニクリナイト
型Ｂｉ２Ｍｏｂ６を合成することができる。In the method of the present invention, instead of γ'-Bi2Moo, B, which generates Bi2O3, Mob, by thermal decomposition is used as a compound and Mo compound in a molar ratio of Bi2O,:MoO5 of 1.
Coniclinite-type Bi2Mob6 can be similarly synthesized by using a mixture at a ratio of :1.
その代表的な化合物としては、例えば、Ｂ１化合物とし
ては、Ｂｉ（Ｎｏ、）、・５Ｈ２０、Ｂｉｂ２（Ｎｏ３
）・５Ｈ２０゜あるいはＢｉ（ＯＨ）３が挙げられ、Ｍ
ｏ化合物としては（ＮＨ４）６ＭＯ７０２ａ・４Ｈ２０
が挙げられる。Typical compounds include, for example, B1 compounds include Bi(No, ), 5H20, Bib2(No3
)・5H20° or Bi(OH)3, M
o compound is (NH4)6MO702a・4H20
can be mentioned.
（ＮＨ４）６ＭＯ７０２４・４Ｈ２０とＢｉ（ＯＨ）３
の酸化物としてのモル比で１：１の混合物を使用した場
合における反応が完全に進行する温度、圧力及び加熱時
間を示すと次の通りであった。(NH4)6MO7024・4H20 and Bi(OH)3
The temperature, pressure, and heating time for the reaction to proceed completely when a mixture with a molar ratio of 1:1 as an oxide was used was as follows.
１ ’／ノ
第 ２ 表
温度じＣ） 圧力（Ｋｙ／ｃｍ２） 時間（ｈ）３５０
１５００ １４４
４００ ９１
５００ ２４
５５０ ３
第１表及び第２表の結果からも、本発明の方法において
は、加熱温度は４００°Ｃ〜６００℃であることが必要
である。４００°Ｃ未満の温度では反応完結時間が非常
にかかり経済的に不利であるか、転移が不能である。ま
た圧力は１５０ Ｋｙ／ｃｍ”以上であることが必要で
、１５０Ｋｙ／Ｃｍ２未満では完全転移ができ難い。1'/no Table 2 Temperature C) Pressure (Ky/cm2) Time (h) 350
1500 144 400 91 500 24 550 3 Also from the results in Tables 1 and 2, in the method of the present invention, the heating temperature needs to be 400°C to 600°C. At temperatures below 400°C, the reaction takes too long to complete and is economically disadvantageous, or the transformation is impossible. Further, the pressure needs to be 150 Ky/cm" or more, and if it is less than 150 Ky/cm2, it is difficult to achieve complete transition.
実施例
実施例１゜
粉末状のγ’−Ｂｉ２Ｍｏｂ６を白金管中に封入して、
圧力容器中に静置した。圧力容器を１５００ Ｋｙ／ｃ
＋ｎ２の一定圧力に保ちながら、電気炉にて５５０℃で
２時間加熱したのち、冷却した。得られたものは黄（９
）
（８）
慣色のコニクリナイト型Ｂｉ２Ｍｏｂ６であった。Examples Example 1゜Powdered γ'-Bi2Mob6 was sealed in a platinum tube,
It was placed in a pressure vessel. Pressure vessel 1500 Ky/c
The mixture was heated at 550° C. for 2 hours in an electric furnace while maintaining a constant pressure of +n2, and then cooled. The obtained product is yellow (9
) (8) It was a conventional color coniclinite type Bi2Mob6.
実施例２゜
（ＮＨ４）６ＭＯ７０２４・４Ｈ２０の粉末とＢｉ（Ｏ
ＨＪ、の粉末をモル比で１：１４の割合で混合した。該
混合物を白金管中に封入ｔ７、圧力容器中に静置した。Example 2゜(NH4)6MO7024・4H20 powder and Bi(O
Powders of HJ were mixed at a molar ratio of 1:14. The mixture was sealed in a platinum tube (t7) and left in a pressure vessel.
圧力容器を１５００ Ｋ７７ｃｍ２の一定圧力に保ちな
がら、電気炉にて５５０°Ｃで３時間加熱した。常圧で
さらに１時間加熱し乾燥した。得られたものは黄緑色の
コニクリナイト型Ｂ１２Ｍ００６であった。The pressure vessel was heated at 550°C for 3 hours in an electric furnace while maintaining a constant pressure of 1500K77cm2. The mixture was further dried by heating at normal pressure for 1 hour. What was obtained was yellow-green coniclinite type B12M006.
発明の効果
本発明の方法によると、圧力を加えながら加熱する簡単
な方法で、γ′型Ｂ土２ ＭｏＯ６からコニクリナイト
型Ｂ１２Ｍ００６への転移を不可能とされていたものを
容易にしかも比較的低温で転移可能とかし得、また、熱
分解によυそれぞれＢｉ２Ｏ３，Ｍｏｂ、を生成するＢ
ｉ化合物とＭｏ化合物の混合物を使用して、比較的低温
で容易にコニクリナイト型Ｂｉ２Ｍｏｂ６を合成し得ら
れる優れた効果を有する。Effects of the Invention According to the method of the present invention, the transformation from γ' type B soil 2 MoO6 to coniclinite type B12M006, which was thought to be impossible, can be easily performed at a relatively low temperature by heating while applying pressure. B can be transferred by pyrolysis and generates υBi2O3 and Mob, respectively.
Coniclinite-type Bi2Mob6 can be easily synthesized at a relatively low temperature using a mixture of the i compound and the Mo compound, resulting in excellent effects.
第１図はコニクリナイト型Ｂ１２Ｍ００６とγ′型（１
０）
１＋ｌｉ％↓２Ｍｏｂ６についての圧力一温度平衡図を
示し、Ａ：コニクリナイト型ＢｉＭＯ０６の安定領域、
Ｂ：γ′型Ｂ１２Ｍｏ０６ノ安定領域、
第２図は本発明の方法による転移によりコニクリナイト
型Ｂ１２Ｍ００６を生成することができる温度−圧力範
囲を示す図である。
斜線で囲まれた領域Ａ：γ′型からコニクリナイト型へ
の転移が１２０時間以内に行われる範囲。
（１１）
第 １ 図Figure 1 shows coniclinite type B12M006 and γ' type (1
0) Shows the pressure-temperature equilibrium diagram for 1+li%↓2Mob6, A: stability region of coniclinite-type BiMO06,
B: Stability region of γ' type B12Mo06. FIG. 2 is a diagram showing the temperature-pressure range in which coniclinite type B12M006 can be produced by transformation according to the method of the present invention. Area A surrounded by diagonal lines: A range where the transition from γ' type to coniclinite type occurs within 120 hours. (11) Figure 1
Claims (1)
５を生成するＢ１化合物と熱分解によりＭｏｏ３を生成
するＭｏ化合物の粉末をＢｉ２Ｏ，： Ｍｏｂ、のモル
比で１：１の割合で混合した混合物を１５０Ｋｙ／ｃｙ
ｎ２以上に加圧し寿がら４００〜６００°Ｃに加熱する
ことを特徴とするコニクリナイト型Ｂ１２Ｗｏｏ６の合
成法。t γ′ type B12M0O6 or Bi2O by thermal decomposition
150 Ky/cy
A method for synthesizing coniclinite type B12Woo6, which is characterized by pressurizing to n2 or more and heating to 400 to 600°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59122773A JPS60264328A (en) | 1984-06-14 | 1984-06-14 | Synthesis of bi2moo6 of koechlinite type |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59122773A JPS60264328A (en) | 1984-06-14 | 1984-06-14 | Synthesis of bi2moo6 of koechlinite type |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60264328A true JPS60264328A (en) | 1985-12-27 |
| JPS6316339B2 JPS6316339B2 (en) | 1988-04-08 |
Family
ID=14844254
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59122773A Granted JPS60264328A (en) | 1984-06-14 | 1984-06-14 | Synthesis of bi2moo6 of koechlinite type |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60264328A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437470A (en) * | 2014-11-06 | 2015-03-25 | 上海市纳米科技与产业发展促进中心 | Homogeneous yolk-shell structure Bi2MoO6 microsphere as well as preparation method and application thereof |
-
1984
- 1984-06-14 JP JP59122773A patent/JPS60264328A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104437470A (en) * | 2014-11-06 | 2015-03-25 | 上海市纳米科技与产业发展促进中心 | Homogeneous yolk-shell structure Bi2MoO6 microsphere as well as preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6316339B2 (en) | 1988-04-08 |
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