JPH0114165B2 - - Google Patents
Info
- Publication number
- JPH0114165B2 JPH0114165B2 JP13515180A JP13515180A JPH0114165B2 JP H0114165 B2 JPH0114165 B2 JP H0114165B2 JP 13515180 A JP13515180 A JP 13515180A JP 13515180 A JP13515180 A JP 13515180A JP H0114165 B2 JPH0114165 B2 JP H0114165B2
- Authority
- JP
- Japan
- Prior art keywords
- crystals
- filling rate
- temperature
- aluminum phosphate
- aluminum
- 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
- 239000013078 crystal Substances 0.000 claims description 21
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 15
- 239000011734 sodium Substances 0.000 claims description 14
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007858 starting material Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 5
- 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 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 229910017119 AlPO Inorganic materials 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 238000003786 synthesis reaction Methods 0.000 description 6
- 235000011007 phosphoric acid Nutrition 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018626 Al(OH) Inorganic materials 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- YDHWWBZFRZWVHO-UHFFFAOYSA-N [hydroxy(phosphonooxy)phosphoryl] phosphono hydrogen phosphate Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(=O)OP(O)(O)=O YDHWWBZFRZWVHO-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- WMWXXXSCZVGQAR-UHFFFAOYSA-N dialuminum;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[O-2].[Al+3].[Al+3] WMWXXXSCZVGQAR-UHFFFAOYSA-N 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- BNIILDVGGAEEIG-UHFFFAOYSA-L disodium hydrogen phosphate Chemical compound [Na+].[Na+].OP([O-])([O-])=O BNIILDVGGAEEIG-UHFFFAOYSA-L 0.000 description 1
- 229910000397 disodium phosphate Inorganic materials 0.000 description 1
- 235000019800 disodium phosphate Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000002783 friction material Substances 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
- 239000000203 mixture Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 description 1
- 150000004685 tetrahydrates Chemical class 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-N triphosphoric acid Chemical compound OP(O)(=O)OP(O)(=O)OP(O)(O)=O UNXRWKVEANCORM-UHFFFAOYSA-N 0.000 description 1
- 229940048102 triphosphoric acid Drugs 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は針状リン酸アルミニウム結晶、とくに
長さと径の比が５以上となるような針状リン酸ア
ルミニウム結晶の製造法に関するものである。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to a method for producing acicular aluminum phosphate crystals, particularly acicular aluminum phosphate crystals having a length-to-diameter ratio of 5 or more. .
従来、リン酸アルミニウムはアルミニウム含有
物質とリン酸質物質からなる混合物を加熱処理す
るか、またはオートクレーブ処理することによつ
て得られているが、いずれも塊状結晶で針状結晶
は得られていない。
Conventionally, aluminum phosphate has been obtained by heat-treating or autoclaving a mixture of an aluminum-containing substance and a phosphoric acid substance, but in both cases, only bulk crystals have been obtained, and needle-shaped crystals have not been obtained. .
本発明は上記の問題点を解決するため種々研究
の結果、アルミニウムとナトリウムをNa2O／
Al2O3のモル比で0.5〜1.5の割合で含有する出発
原料にリン酸質物質をP2O5／Al2O3のモル比が１
〜３となるように混合し、充てん率20〜70％、温
度200〜500℃の条件でオートクレーブ処理即ち水
熱処理することによつて針状のリン酸アルミニウ
ム結晶を得ることに成功したものである。
In order to solve the above-mentioned problems, the present invention was developed as a result of various studies, and as a result of various researches, aluminum and sodium were converted into Na 2 O/
A phosphoric acid substance is added to the starting material containing Al 2 O 3 at a molar ratio of 0.5 to 1.5, and the P 2 O 5 /Al 2 O 3 molar ratio is 1.
We succeeded in obtaining acicular aluminum phosphate crystals by mixing the aluminum phosphates in an autoclave or hydrothermal treatment at a filling rate of 20 to 70% and a temperature of 200 to 500°C. .
すなわち、本発明は上記のナトリウムを含有す
る原料の混合条件と、オートクレーブ処理条件に
よつて、リン酸アルミニウム結晶の成長速度をＣ
軸方向に大きくなるように成長癖を制御して針状
結晶を得ることに成功したものである。 That is, the present invention improves the growth rate of aluminum phosphate crystals by adjusting the mixing conditions of the above-mentioned sodium-containing raw materials and the autoclaving conditions.
We succeeded in obtaining needle-shaped crystals by controlling the growth habit so that they become larger in the axial direction.
本発明において使用する出発原料の内Al原料
としては酸化アルミニウム（Al2O3）、酸化アル
ミニウムの水和物（Al2O3・H2O，Al2O3・
3H2O）など，Na原料としては金属Na，酸化ナ
トリウム（Na2O），水酸化ナトリウム（NaOH）
など，Ｐ原料としては五酸化ニリン（P2O5）お
よびそれが水和してできる酸（メタリン酸，ピロ
リン酸，オルトリン酸，三リン酸，四リン酸）な
ど，さらにはAl，Na，Ｐを２種以上含む原料と
してはリン酸水素ナトリウム（Na2HPO4，
NaH2PO4など）とその水和物AlPO4・nH2Oな
どが使用できる。 Among the starting materials used in the present invention, Al raw materials include aluminum oxide (Al 2 O 3 ) and aluminum oxide hydrates (Al 2 O 3 ·H 2 O, Al 2 O 3 ·
Na raw materials include metallic Na, sodium oxide (Na 2 O ), and sodium hydroxide (NaOH).
Examples of P raw materials include niline pentoxide (P 2 O 5 ) and the acids formed by its hydration (metaphosphoric acid, pyrophosphoric acid, orthophosphoric acid, triphosphoric acid, tetraphosphoric acid), as well as Al, Na, Raw materials containing two or more types of P include sodium hydrogen phosphate (Na 2 HPO 4 ,
NaH 2 PO 4 etc.) and its hydrate AlPO 4 .nH 2 O etc. can be used.
オートクレーブ処理（水熱処理）を行うのは、
従来法と同様、水の存在を必要とするからで、原
料の水に対する濃度範囲は酸化物換算で５〜
70wt％である。 Autoclave treatment (hydrothermal treatment) is performed by
This is because, like the conventional method, the presence of water is required, and the concentration range of the raw material in water is 5 to 5 in terms of oxides.
It is 70wt%.
原料が5wt％より少ない場合は生成物は塊状結
晶となり、70wt％を越える場合は非晶質しか得
られず、針状結晶は得られない。 If the raw material content is less than 5 wt%, the product will be bulk crystals, and if it exceeds 70 wt%, only amorphous crystals will be obtained, and needle-shaped crystals will not be obtained.
本発明において、上記のように数値を限定する
のは、それ以外の範囲では、AlPO4自体が合成で
きないか、あるいはできたとしても塊状結晶であ
り、針状結晶が合成できないからである。 In the present invention, the numerical values are limited as described above because in other ranges, AlPO 4 itself cannot be synthesized, or even if AlPO 4 can be synthesized, it will be lumpy crystals and needle-shaped crystals cannot be synthesized.
すなわち温度200℃以下，充てん率20％以下で
はAlPO4水和物または非晶質が、温度500℃以上、
充てん率70％以上では塊状のAlPO4結晶しか得ら
れない。 In other words, when the temperature is below 200℃ and the filling rate is below 20%, AlPO tetrahydrate or amorphous is present, but when the temperature is above 500℃,
At a filling rate of 70% or more, only massive AlPO 4 crystals can be obtained.
なお、反応時の圧力は、周知のように充てん率
と温度によつて決まるものであるが、上記の充て
ん率及び温度範囲の場合は、その圧力の範囲は10
〜2000atmである。 As is well known, the pressure during the reaction is determined by the filling rate and temperature, but in the case of the above filling rate and temperature range, the pressure range is 10
~2000 atm.
また反応時間は１時間以上要し、発明者等の実
験では、１時間以下では針状AlPO4結晶は得られ
なかつた。 Further, the reaction time required was 1 hour or more, and according to the experiments conducted by the inventors, needle-shaped AlPO 4 crystals could not be obtained in less than 1 hour.
以下、本発明の実施例を示すが、本発明は下記
した例に限定されるものではない。 Examples of the present invention will be shown below, but the present invention is not limited to the examples described below.
（実施例 １）
Al（OH）3紛末7.8ｇに5N NaOH溶液10mlをか
く拌混合して得られた出発原料に9M H3PO4溶
液20mlを配合して合成用原料とした。この場合の
Na2O／Al2O3は0.5、P2O5／Al2O3は1.8となる。
この合成用原料を下記の条件で48時間オートクレ
ーブ処理により合成した結果長さ200〜500μm，
径10〜15μmの針状リン酸アルミニウム結晶が10
ｇ得られた。(Example 1) A starting material obtained by stirring and mixing 7.8 g of Al(OH) 3 powder with 10 ml of a 5N NaOH solution was mixed with 20 ml of a 9M H 3 PO 4 solution to obtain a raw material for synthesis. In this case
Na 2 O / Al 2 O 3 is 0.5, and P 2 O 5 /Al 2 O 3 is 1.8.
This raw material for synthesis was synthesized by autoclaving for 48 hours under the following conditions, resulting in a length of 200 to 500 μm.
10 acicular aluminum phosphate crystals with a diameter of 10-15 μm
g was obtained.
オートクレーブ処理条件 充てん率 30％ 温 度 400℃ なお、容器は銀製のものを使用した。 Autoclave processing conditions Filling rate 30% Temperature 400℃ Note that the container used was made of silver.
（実施例 ２）
AlPO4紛末12.2ｇに10N NaOH溶液10mlをか
く拌混合して得られた出発原料に9M H3PO4溶
液20mlを配合して合成用原料とした。この場合の
Na2O／Al2O3は、1.0、P2O5／Al2O3は1.8とな
る。この合成用原料を下記の条件で48時間オート
クレーブ処理により合成した結果、長さ100〜
300μm，径10〜20μmの針状リン酸アルミニウム
結晶が５ｇ得られた。(Example 2) A starting material obtained by stirring and mixing 12.2 g of AlPO 4 powder with 10 ml of 10N NaOH solution was mixed with 20 ml of 9M H 3 PO 4 solution to prepare a raw material for synthesis. In this case
Na 2 O / Al 2 O 3 is 1.0, and P 2 O 5 /Al 2 O 3 is 1.8. As a result of synthesizing this raw material for synthesis by autoclaving for 48 hours under the following conditions, the length was 100~
5 g of acicular aluminum phosphate crystals with a diameter of 300 μm and a diameter of 10 to 20 μm were obtained.
オートクレーブ処理条件
充てん率 30％
温 度 400℃
（実施例 ３）
NaAlO2紛末8.2ｇを出発原料として、これに
7M H3PO4溶液30mlを混合して合成用原料とし
た。この場合のNa2O／Al2O3は1.0、P2O5／
Al2O3は2.1となる。 Autoclave treatment conditions Filling rate 30% Temperature 400℃ (Example 3) Using 8.2g of NaAlO2 powder as a starting material,
30 ml of 7M H 3 PO 4 solution was mixed and used as a raw material for synthesis. In this case, Na 2 O / Al 2 O 3 is 1.0, P 2 O 5 /
Al 2 O 3 is 2.1.
この合成用原料を下記の条件で48時間オートク
レーブ処理により合成した結果、長さ100〜
500μm，径10〜15μmの針状リン酸アルミニウム
結晶が６ｇ得られた。 As a result of synthesizing this raw material for synthesis by autoclaving for 48 hours under the following conditions, the length was 100~
6 g of acicular aluminum phosphate crystals with a diameter of 500 μm and a diameter of 10 to 15 μm were obtained.
オートクレーブ処理条件
充てん率 30％
温 度 350℃
以上述べたごとく、従来塊状のものしか合成で
きなかつたリン酸アルミニウムは、アルミニウム
とナトリウムをNa2O／Al2O3のモル比で0.5〜1.5
の割合で含有する出発原料にリン酸質物質を
P2O5／Al2O3のモル比が１〜３となるように混合
し、充てん率20〜70％、温度200〜500℃の条件で
オートクレーブ処理することによつて針状のもの
が合成される。 Autoclave treatment conditions Filling rate: 30% Temperature: 350°C As mentioned above, aluminum phosphate, which could only be synthesized in bulk form, is produced by combining aluminum and sodium in a molar ratio of Na 2 O / Al 2 O 3 of 0.5 to 1.5.
Phosphate substances are added to the starting materials containing a proportion of
By mixing P 2 O 5 /Al 2 O 3 at a molar ratio of 1 to 3 and autoclaving at a filling rate of 20 to 70% and a temperature of 200 to 500°C, needle-like particles are formed. be synthesized.
この場合、実施例でも明らかなごとく、原料成
分の混合割合とオートクレーブ条件が重要であ
り、原料に使用する物質は限定されない。なお、
本発明の実施例において得られた結晶は単結晶で
あることが確認された。 In this case, as is clear from the examples, the mixing ratio of raw material components and autoclave conditions are important, and the substances used as raw materials are not limited. In addition,
It was confirmed that the crystals obtained in the examples of the present invention were single crystals.
本発明の構成により得られる針状リン酸アルミ
ニウム結晶は、耐熱性を利用して断熱材として、
またアスベスト代替としての摩擦材や隔膜材、触
媒担体あるいはその補強材としての利用が可能で
あり、またその他の応用分野たとえばAlPO4の圧
電性を利用したものなど、きはめて多面的な活用
が可能であると確信する。 The acicular aluminum phosphate crystal obtained by the structure of the present invention can be used as a heat insulating material by utilizing its heat resistance.
In addition, it can be used as a friction material, diaphragm material, catalyst carrier, or its reinforcement material as an alternative to asbestos, and it can also be used in many other fields, such as those that utilize the piezoelectric properties of AlPO4 . I am convinced that it is possible.
Claims (1)
のモル比で0.5〜1.5の割合で含有する出発原料に
リン酸物質をP2O5／Al2O3のモル比が１〜３とな
るように混合し、充てん率20〜70％、温度200〜
500℃の条件でオートクレーブ処理することを特
徴とする針状リン酸アルミニウム結晶の製造法。1 Aluminum and sodium are converted into Na 2 O/Al 2 O 3
A phosphoric acid substance is mixed with a starting material containing a molar ratio of 0.5 to 1.5 so that the molar ratio of P 2 O 5 /Al 2 O 3 is 1 to 3, the filling rate is 20 to 70%, and the temperature is 200～
A method for producing acicular aluminum phosphate crystals, which is characterized by autoclave treatment at 500°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13515180A JPS5761607A (en) | 1980-09-30 | 1980-09-30 | Preparation of needle-like crystal of aluminum phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13515180A JPS5761607A (en) | 1980-09-30 | 1980-09-30 | Preparation of needle-like crystal of aluminum phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5761607A JPS5761607A (en) | 1982-04-14 |
| JPH0114165B2 true JPH0114165B2 (en) | 1989-03-09 |
Family
ID=15145001
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13515180A Granted JPS5761607A (en) | 1980-09-30 | 1980-09-30 | Preparation of needle-like crystal of aluminum phosphate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5761607A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2517187Y2 (en) * | 1989-12-19 | 1996-11-13 | 日本輸送機株式会社 | Obstacle detection device for work trolley with lifting device |
| US8025725B2 (en) * | 2006-12-13 | 2011-09-27 | Taki Chemical Co., Ltd. | Temperature-sensitive aluminum phosphate solution, a process for producing the same and the use thereof |
-
1980
- 1980-09-30 JP JP13515180A patent/JPS5761607A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5761607A (en) | 1982-04-14 |
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