JPH0449484B2 - - Google Patents
Info
- Publication number
- JPH0449484B2 JPH0449484B2 JP2283485A JP2283485A JPH0449484B2 JP H0449484 B2 JPH0449484 B2 JP H0449484B2 JP 2283485 A JP2283485 A JP 2283485A JP 2283485 A JP2283485 A JP 2283485A JP H0449484 B2 JPH0449484 B2 JP H0449484B2
- Authority
- JP
- Japan
- Prior art keywords
- alkyl group
- silicate
- carbon atoms
- aluminum
- general formula
- 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
- 239000000843 powder Substances 0.000 claims description 22
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- -1 silicon alkoxide Chemical class 0.000 claims description 16
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 14
- 229910052863 mullite Inorganic materials 0.000 claims description 14
- 238000010992 reflux Methods 0.000 claims description 13
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 10
- 125000000217 alkyl group Chemical group 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 claims description 5
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 4
- 239000003125 aqueous solvent Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 235000012239 silicon dioxide Nutrition 0.000 claims description 2
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 claims description 2
- ZUEKXCXHTXJYAR-UHFFFAOYSA-N tetrapropan-2-yl silicate Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)OC(C)C ZUEKXCXHTXJYAR-UHFFFAOYSA-N 0.000 claims description 2
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 125000005234 alkyl aluminium group Chemical group 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000000926 separation method Methods 0.000 claims 1
- 238000005245 sintering Methods 0.000 claims 1
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 230000007062 hydrolysis Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001879 gelation Methods 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- JHUUPUMBZGWODW-UHFFFAOYSA-N 3,6-dihydro-1,2-dioxine Chemical compound C1OOCC=C1 JHUUPUMBZGWODW-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 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
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 229940115440 aluminum sodium silicate Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- AZWXAPCAJCYGIA-UHFFFAOYSA-N bis(2-methylpropyl)alumane Chemical compound CC(C)C[AlH]CC(C)C AZWXAPCAJCYGIA-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- HJXBDPDUCXORKZ-UHFFFAOYSA-N diethylalumane Chemical compound CC[AlH]CC HJXBDPDUCXORKZ-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N methoxybenzene Substances CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- SQBBHCOIQXKPHL-UHFFFAOYSA-N tributylalumane Chemical compound CCCC[Al](CCCC)CCCC SQBBHCOIQXKPHL-UHFFFAOYSA-N 0.000 description 1
- ORYGRKHDLWYTKX-UHFFFAOYSA-N trihexylalumane Chemical compound CCCCCC[Al](CCCCCC)CCCCCC ORYGRKHDLWYTKX-UHFFFAOYSA-N 0.000 description 1
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 1
- LFXVBWRMVZPLFK-UHFFFAOYSA-N trioctylalumane Chemical compound CCCCCCCC[Al](CCCCCCCC)CCCCCCCC LFXVBWRMVZPLFK-UHFFFAOYSA-N 0.000 description 1
- CNWZYDSEVLFSMS-UHFFFAOYSA-N tripropylalumane Chemical compound CCC[Al](CCC)CCC CNWZYDSEVLFSMS-UHFFFAOYSA-N 0.000 description 1
- MLDSMTVYPPIXMZ-UHFFFAOYSA-N tris(4-methylpentyl)alumane Chemical compound CC(C)CCC[Al](CCCC(C)C)CCCC(C)C MLDSMTVYPPIXMZ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Landscapes
- Silicates, Zeolites, And Molecular Sieves (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、高純度で且つ凝集のない微細なムラ
イト粉末の製造法に関するものである。ムライト
粉末は、優れた耐熱性を有するため、耐熱材料と
してのセラミツク原料粉末として有用な化合物で
ある。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing fine mullite powder with high purity and no agglomeration. Since mullite powder has excellent heat resistance, it is a compound useful as a ceramic raw material powder as a heat-resistant material.
（従来の技術〕
従来、その製造法として次の方法が知られてい
るが、それらのいづれの方法によつても何等かの
欠点がある。(Prior Art) Conventionally, the following methods have been known as manufacturing methods, but all of these methods have some drawbacks.
(1) 粘土（カオリン）と水酸化アルミニウム（又
はアルミナ）を粉砕混合し加熱する方法、又は
硫酸アルミニウム、ケイ酸ソーダと硫酸ソーダ
を混合し加熱する方法などが用いられている
が、この方法では生成物にカリウム、ナトリウ
ムが入り易いため高純度の粉末が得られない。(1) Methods such as pulverizing and mixing clay (kaolin) and aluminum hydroxide (or alumina) and heating them, or mixing and heating aluminum sulfate, sodium silicate and sodium sulfate are used. High purity powder cannot be obtained because potassium and sodium easily enter the product.
(2) アルミニウムアルコキシドとシリコンアルコ
キシドを混合し加水分解する方法、又はアルミ
ナゾルとシリカゾルを混合し加熱する方法等が
用いられているが、この方法では凝集粒子とな
り易く成形性に劣つた粉末となり、粉砕、解砕
又はふるい分けの行程を必要とする。(2) Methods such as mixing aluminum alkoxide and silicon alkoxide and hydrolyzing them, or mixing alumina sol and silica sol and heating them, etc., are used, but these methods tend to aggregate particles and result in powder with poor moldability, resulting in pulverization. , requiring a crushing or sieving process.
本発明の高純度で且つ凝集のない微細なムライ
ト粉末の製造法は、これらの従来の欠点を改善す
るためになされたものである。
The method of producing fine mullite powder with high purity and no agglomeration according to the present invention has been developed in order to improve these conventional drawbacks.
本発明も要旨は、一般式R2ＡR′で示される
アルキルアルミニウムと一般式Si（OR）4で示され
るシリコンアルコキシドを生成するケイ酸アルミ
ニウムがムライト組成になるように予め調整して
混合加熱し、しかる後非水溶媒中で加水分解して
微細なケイ酸アルミニウムを生成し、焼成するこ
とを特徴とする高純度ムライト粉末の製造法にあ
る。更に詳しくは、アルキルアルミニウム化合物
とシリコンアルコキシドを予めムライト組成に調
整後混合して80℃〜200℃で加熱還流せしめ、そ
の還流溶液と予めアンモニア水を加えてPHを調整
したイオン交換水を非水溶媒中に徐々に同時添加
して加水分解することにより、高純度でしかも凝
集のない微細なムライト粉末を製造する方法にあ
る。
The gist of the present invention is that aluminum alkyl represented by the general formula R 2 AR' and aluminum silicate which produces silicon alkoxide represented by the general formula Si(OR) 4 are mixed and heated so that they have a mullite composition. , followed by hydrolysis in a non-aqueous solvent to produce fine aluminum silicate, which is then fired. More specifically, an alkyl aluminum compound and a silicon alkoxide are mixed in advance to have a mullite composition, heated to reflux at 80°C to 200°C, and the refluxed solution and ion-exchanged water, the pH of which has been adjusted by adding ammonia water, are mixed into a non-aqueous solution. The present invention is a method for producing fine mullite powder with high purity and no agglomeration by gradually and simultaneously adding it to a solvent and hydrolyzing it.
本発明を更に詳しく説明すれば、アルミナ源と
しては一般式R2ＡR′（但し、Ｒは炭素数１〜20
のアルキル基、R′は炭素数１〜８のアルキル基
または水素原子）で示されるアルキルアルミニウ
ム化合物、例えばトリメチルアルミニウム、トリ
エチルアルミニウム、トリ−ｎ−プロピルアルミ
ニウム、トリ−iso−ブチルアルミニウム、トリ
−ｎ−ブチルアルミニウム、トリ−iso−ヘキシ
ルアルミニウム、トリ−ｎ−ヘキシルアルミニウ
ム、トリ−ｎ−オクチルアルミニウム、トリイソ
プレニルアルミニウム、ジエチルアルミニウムハ
イドライド、ジ−iso−ブチルアルミニウムハイ
ドライド等である。シリカ源としては一般式Si
（OR）4（但し、Ｒは炭素数１〜20のアルキル基）
で示されるシリコンアルコキシド、例えばメチル
シリケート、エチルシリケート、イソプロピルシ
リケート、ブチルシリケート等である。このアル
キルアルミニウム化合物とシリコンアルコキシド
とをアルミナとケイ酸の割合が５：２〜1.5：１
になるように予め調整して混合し、この混合溶液
を攪拌しながら80〜200℃の温度に好ましくは100
℃〜150℃の温度に加熱して還流させることによ
り均一化する。還流反応を行なわずに、加水分解
すると、アルミナ源とシリカ源の結晶化速度の違
いにより得られる反応生成物は二層に分離し、均
一性に劣るため、十分還流させることが必要であ
る。 To explain the present invention in more detail, the alumina source has the general formula R 2 AR' (where R has 1 to 20 carbon atoms).
alkyl group, R' is an alkyl group having 1 to 8 carbon atoms or a hydrogen atom), such as trimethylaluminum, triethylaluminum, tri-n-propylaluminum, tri-iso-butylaluminum, tri-n -butylaluminum, tri-iso-hexylaluminum, tri-n-hexylaluminum, tri-n-octylaluminum, triisoprenylaluminum, diethylaluminum hydride, di-iso-butylaluminum hydride, and the like. As a silica source, the general formula Si
(OR) 4 (However, R is an alkyl group having 1 to 20 carbon atoms)
Examples of silicon alkoxides include methyl silicate, ethyl silicate, isopropyl silicate, butyl silicate, and the like. This alkylaluminium compound and silicon alkoxide are mixed at a ratio of alumina and silicic acid of 5:2 to 1.5:1.
Adjust the mixture in advance so that
Homogenize by heating to a temperature between 150°C and reflux. If hydrolysis is performed without carrying out a reflux reaction, the reaction product obtained will separate into two layers due to the difference in crystallization rate between the alumina source and the silica source, resulting in poor homogeneity, so it is necessary to carry out sufficient reflux.
次に、この還流溶液と予めアンモニア水でPH＝
８以上、好ましくはPH＝11以上に調整したイオン
交換水を還流溶液に対し、1.0〜5.0モル倍量好ま
しくは２〜３モル倍量を非水溶媒中に一定速度で
徐々に同時に添加し、加水分解する。この場合非
水溶媒としては炭化水素系溶媒例えば、ヘキサ
ン、ヘプタン等、芳香族炭化水素系溶媒例えばベ
ンゼン、トルエン、キシレン等、エーテル系溶媒
例えば１，４−ジオキサン、ジエチルエーテル、
テトラヒドロフラン、アニソール等、第三級アミ
ン系溶媒例えばピリジン、トリエチルアミン等を
単独又は混合して用いることができ、特に限定さ
れるものではなが、好ましくは、トルエンが良
い。又、添加方法であるが還流溶液を先ず非水溶
媒で希釈し、それにPH調整したイオン交換水を添
加する方法もあるが、還流溶液とPH調整したイオ
ン交換水を非水溶媒中に一定速度で徐々に同時添
加し、一気にゲル化を生じさせないよう粘度を制
御することにより、微細なケイ酸アルミニウムの
ゾルを生成することが望ましい。この方法で得た
ゾルから蒸留操作により、溶媒を除去した後、50
℃〜100℃温度で減圧乾燥し微細なケイ酸アルミ
ニウムの粉末が得られる。 Next, this refluxing solution and ammonia water were added in advance to pH=
Gradually and simultaneously add 1.0 to 5.0 moles, preferably 2 to 3 moles of ion-exchanged water adjusted to a pH of 8 or higher, preferably 11 or higher, into a non-aqueous solvent at a constant rate, to the refluxing solution, Hydrolyze. In this case, the nonaqueous solvent includes hydrocarbon solvents such as hexane and heptane, aromatic hydrocarbon solvents such as benzene, toluene, and xylene, and ether solvents such as 1,4-dioxane and diethyl ether.
Tetrahydrofuran, anisole, etc., tertiary amine solvents such as pyridine, triethylamine, etc. can be used alone or in combination, and toluene is preferably used, although there are no particular limitations. Another method of addition is to first dilute the refluxing solution with a non-aqueous solvent and then add ion-exchanged water with adjusted pH to it. It is desirable to generate a fine sol of aluminum silicate by gradually adding the aluminum silicate at the same time and controlling the viscosity so as not to cause gelation all at once. After removing the solvent from the sol obtained by this method by distillation,
Fine aluminum silicate powder is obtained by drying under reduced pressure at a temperature of 100°C to 100°C.
この乾燥粉末は、通常30〜40％の程度の水分を
含んでいるので700℃〜1300℃の温度で焼成する
と極めて微細なムライト粉末が生成する。 This dry powder usually contains about 30 to 40% water, so when fired at a temperature of 700°C to 1300°C, extremely fine mullite powder is produced.
本発明により得られるムライト粉末は通常５〜
100m2／ｇの比表面積を有しており、出発原料を
予め精製することにより純度99.999％以上の粉末
を得ることも可能である。 The mullite powder obtained by the present invention usually has a
It has a specific surface area of 100 m 2 /g, and it is possible to obtain a powder with a purity of 99.999% or more by refining the starting material in advance.
尚本発明の製造法において微細なムライト粉末
を得るには加水分解において、ゲル化濃度を制御
することが最も重要であり、この製造方法によ
り、高純度且つ微細なムライト粉末が得られ、各
種窯業用に広く用いることができ、安定して供給
できる産業上極めて有用な方法である。 In addition, in order to obtain fine mullite powder in the production method of the present invention, it is most important to control the gelation concentration during hydrolysis.This production method yields highly pure and fine mullite powder, which is suitable for various ceramic industries. It is an industrially extremely useful method that can be widely used for various purposes and can be stably supplied.
（実施例）
次に本発明を実施例で説明するが、これに限定
されるものではない。(Example) Next, the present invention will be explained using examples, but the present invention is not limited thereto.
実施例 １
攪拌装置及び還流冷却器を備えた２４ツロフ
ラスコにN2雰囲気下でトリエチルアルミニウム
830mlを仕込み、これを攪拌しながら室温でエチ
ルシリケート470mlを徐々に添加した。添加終了
後、温度を120℃に昇温し、約５時間還流反応を
行なつた後、室温まで放冷した。次に２セパラ
ブルフラスコにN2雰囲気下で１，４−ジオキサ
ン315mlとトルエン520mlの混合溶媒を仕込み攪拌
しながら、前述のトリエチルアルミニウムとエチ
ルシリケートの還流反応をした溶液130mlと予め
アンモニア水でPH＝11.5に調整したイオン交換水
42mlをゆつくりと同時に添加し、加水分解を行つ
た。そのときの添加速度は還流反応溶液が16ml／
Hr，PH調整イオン交換水が５ml／Hrで、加水分
解反応温度は10℃に保持した。添加終了後、完全
に加水分解するため、更に２時間攪拌を続けた。
加水分解によつて得られた反応生成物をロータリ
ーエバポレーターを使用して溶媒を分離後、70℃
で10時間減圧乾燥することにより、微細なケイ酸
アルミニウムの粉末が得られた。この粉末は100
〜500m2／ｇの比表面積を有し、0.3〜0.7ｇ／ml
の容積密度を有していた。Example 1 Triethylaluminum was added under an atmosphere of N2 to a 24 tube flask equipped with a stirrer and a reflux condenser.
830 ml of ethyl silicate was charged, and 470 ml of ethyl silicate was gradually added thereto at room temperature while stirring. After the addition was completed, the temperature was raised to 120°C, a reflux reaction was carried out for about 5 hours, and then the mixture was allowed to cool to room temperature. Next, a mixed solvent of 315 ml of 1,4-dioxane and 520 ml of toluene was charged into a two-separable flask under an N2 atmosphere, and while stirring, 130 ml of the above-mentioned reflux reaction solution of triethyl aluminum and ethyl silicate was mixed with aqueous ammonia to PH. = Ion exchange water adjusted to 11.5
42 ml was added at the same time as the loosening to perform hydrolysis. At that time, the addition rate was 16ml/16ml of the refluxing reaction solution.
Hr, pH adjusted ion exchange water was used at 5 ml/Hr, and the hydrolysis reaction temperature was maintained at 10°C. After the addition was complete, stirring was continued for an additional 2 hours to ensure complete hydrolysis.
After separating the solvent from the reaction product obtained by hydrolysis using a rotary evaporator, it was heated to 70°C.
By drying under reduced pressure for 10 hours, fine aluminum silicate powder was obtained. This powder is 100
It has a specific surface area of ~500m 2 /g and 0.3-0.7g/ml
It had a volume density of .
このケイ酸アルミニウムを大気中において1200
℃で２時間焼成し、微細なムライト粉末を得た。
このムライト粉末はSEM観察により平均粒径
0.1μの凝集のない球状粒子であり、比表面積は10
〜20m2／ｇであつた。 This aluminum silicate is exposed to 1200
It was fired at ℃ for 2 hours to obtain fine mullite powder.
The average particle size of this mullite powder was determined by SEM observation.
Spherical particles with no agglomeration of 0.1μ and a specific surface area of 10
It was ~20m 2 /g.
実施例 ２
トリエチルアルミニウム83mlとエチルシリケー
ト47mlとを室温で単に混合攪拌した混合溶液130
mlと予めアンモニア水でPH＝11.5に調整したイオ
ン交換水42mlとを１，４−ジオキサン315mlとト
ルエン520mlの混合溶媒中に一定速度で徐々に同
時添加し加水分解を行つて生成したスラリーを静
定したところ、得た反応生成物は二層に分離し
た。このスラリーを乾燥して得た粉体の化学組成
には、バラツキを生じた。Example 2 Mixed solution 130 in which 83 ml of triethyl aluminum and 47 ml of ethyl silicate were simply mixed and stirred at room temperature.
ml and 42 ml of ion-exchanged water, which had been adjusted to pH=11.5 with aqueous ammonia, were gradually and simultaneously added at a constant rate to a mixed solvent of 315 ml of 1,4-dioxane and 520 ml of toluene, and the resulting slurry was hydrolyzed. Upon determination, the obtained reaction product was separated into two layers. The chemical composition of the powder obtained by drying this slurry varied.
実施例 ３
実施例１において調整した還流溶液130mlを１，
４−ジオキサン315mlとトルエン520mlの混合溶媒
で希釈し、これにPH＝11.5に調整したイオン交換
水42mlを５ml／Hrの速度でゆつくりと添加し加
水分解を行つた。このとき10〜15ml添加付近で急
激なゲル化が起り一時的に粘度の上昇が見られ
た。この方法により得られたケイ酸アルミニウム
の粉末は、一次粒子は微細であるが固く凝集して
おり成形性に劣つた粉体であつた。Example 3 130 ml of the reflux solution prepared in Example 1 was
The mixture was diluted with a mixed solvent of 315 ml of 4-dioxane and 520 ml of toluene, and 42 ml of ion-exchanged water adjusted to pH=11.5 was slowly added thereto at a rate of 5 ml/hr for hydrolysis. At this time, rapid gelation occurred near the addition of 10 to 15 ml, and a temporary increase in viscosity was observed. The aluminum silicate powder obtained by this method had fine primary particles but was tightly aggregated and had poor formability.
Claims (1)
ルキル基、R′は炭素数１〜８のアルキル基また
は水素原子）で示されるアルキルアルミニウム化
合物と、一般式Si（OR）4（但しＲは炭素数１〜20
のアルキル基）で示されるシリコンアルコキシド
とを予めムライト組成に調整後混合加熱し、しか
る後非水溶媒中で加水分解して微細なケイ酸アル
ミニウムを生成し、焼成することを特徴とする高
純度ムライト粉末の製造法。 ２ 一般式R2ＡR′（但しＲは炭素数１〜20のア
ルキル基、R′は炭素数１〜８のアルキル基また
は水素原子）で示されるアルキルアルミニウム化
合物と、一般式Si（OR）4（但しＲは炭素数１〜20
のアルキル基）で示されるシリコンアルコキシド
とを予めムライト組成に調整後混合して加熱還流
を行なわせ、それと予めPH８以上に調整した水と
を非水溶媒中に同時且つゲルが生成しないように
一定速度で添加してケイ酸アルミニウムのゾルを
生成せしめ、しかる後分離、乾燥、焼成して得ら
れる高純度ムライト粉末の製造法。 ３ アルキルアルミニウム化合物がトリエチルア
ルミニウム又はトリイソブチルアルミニウムであ
る特許請求の範囲第１項又は２項記載の方法。 ４ シリコンアルコキシドがエチルシリケート、
イソプロピルシリケート、ブチルシリケートであ
る特許請求の範囲第１項又は２項記載の方法。 ５ アルキルアルミニウム化合物とシリコンアル
コキシドをアルミナとケイ酸の割合が５：２〜
1.5：１になるように調整混合し、この混合溶液
を攪拌しながら80〜200℃に加熱還流して使用す
る特許請求の範囲第１項又は第２項記載の方法。 ６ アンモニア水でPH８以上に調整した水で加水
分解する特許請求の範囲第１項又は第２項記載の
方法。 ７ 非水溶媒としてトルエン、ヘキサン、１，４
−ジオキサンを使用する特許請求の範囲第１項又
は２項記載の方法。[Scope of Claims] 1. Alkylaluminum compounds represented by the general formula R 2 AR' (where R is an alkyl group having 1 to 20 carbon atoms, R' is an alkyl group having 1 to 8 carbon atoms or a hydrogen atom), and general Formula Si(OR) 4 (where R is carbon number 1-20
High-purity aluminum silicate is produced by mixing and heating a silicon alkoxide represented by the alkyl group of Method of manufacturing mullite powder. 2 An alkyl aluminum compound represented by the general formula R 2 AR' (where R is an alkyl group having 1 to 20 carbon atoms, and R' is an alkyl group having 1 to 8 carbon atoms or a hydrogen atom) and a general formula Si(OR) 4 (However, R has 1 to 20 carbon atoms.
A silicon alkoxide represented by (an alkyl group of A method for producing high-purity mullite powder obtained by adding aluminum silicate at a high rate to form a sol, followed by separation, drying, and sintering. 3. The method according to claim 1 or 2, wherein the alkyl aluminum compound is triethyl aluminum or triisobutyl aluminum. 4 Silicon alkoxide is ethyl silicate,
3. The method according to claim 1 or 2, wherein isopropyl silicate or butyl silicate is used. 5 Alkylaluminum compound and silicon alkoxide with a ratio of alumina and silicic acid of 5:2 ~
The method according to claim 1 or 2, wherein the mixed solution is adjusted to a ratio of 1.5:1 and heated to reflux at 80 to 200° C. while stirring. 6. The method according to claim 1 or 2, which comprises hydrolyzing with water adjusted to pH 8 or higher with aqueous ammonia. 7 Toluene, hexane, 1,4 as a non-aqueous solvent
- The method according to claim 1 or 2, in which dioxane is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2283485A JPS61197417A (en) | 1985-02-08 | 1985-02-08 | Production of high-purity mullite powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2283485A JPS61197417A (en) | 1985-02-08 | 1985-02-08 | Production of high-purity mullite powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61197417A JPS61197417A (en) | 1986-09-01 |
| JPH0449484B2 true JPH0449484B2 (en) | 1992-08-11 |
Family
ID=12093730
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2283485A Granted JPS61197417A (en) | 1985-02-08 | 1985-02-08 | Production of high-purity mullite powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61197417A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2139497B1 (en) * | 1997-02-24 | 2000-11-01 | Univ Santiago Compostela | MULLITE PURIFICATION PROCEDURE FOR REDUCING IMPURITIES TO VOLATILE SPECIES. |
-
1985
- 1985-02-08 JP JP2283485A patent/JPS61197417A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61197417A (en) | 1986-09-01 |
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