JPS6350321A - Production of fine-powdery antimony trioxide-hydrated alumina composite composition - Google Patents
Production of fine-powdery antimony trioxide-hydrated alumina composite compositionInfo
- Publication number
- JPS6350321A JPS6350321A JP19043486A JP19043486A JPS6350321A JP S6350321 A JPS6350321 A JP S6350321A JP 19043486 A JP19043486 A JP 19043486A JP 19043486 A JP19043486 A JP 19043486A JP S6350321 A JPS6350321 A JP S6350321A
- Authority
- JP
- Japan
- Prior art keywords
- alkoxide
- iii
- hydrated alumina
- antimony trioxide
- antimony
- 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.)
- Pending
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 32
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 26
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 title claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 19
- -1 antimony (III) alkoxide Chemical class 0.000 claims abstract description 15
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 4
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052782 aluminium Inorganic materials 0.000 abstract description 4
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 150000004820 halides Chemical class 0.000 abstract 1
- 238000006460 hydrolysis reaction Methods 0.000 description 10
- 230000007062 hydrolysis Effects 0.000 description 9
- 239000002244 precipitate Substances 0.000 description 9
- 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 8
- 230000000694 effects Effects 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000000779 smoke Substances 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 239000010419 fine particle Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 description 1
- 150000001463 antimony compounds Chemical class 0.000 description 1
- 229910000410 antimony oxide Inorganic materials 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000002542 deteriorative effect Effects 0.000 description 1
- HHFAWKCIHAUFRX-UHFFFAOYSA-N ethoxide Chemical compound CC[O-] HHFAWKCIHAUFRX-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000010667 large scale reaction Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- OGHBATFHNDZKSO-UHFFFAOYSA-N propan-2-olate Chemical compound CC(C)[O-] OGHBATFHNDZKSO-UHFFFAOYSA-N 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- YPMOSINXXHVZIL-UHFFFAOYSA-N sulfanylideneantimony Chemical compound [Sb]=S YPMOSINXXHVZIL-UHFFFAOYSA-N 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- HYPTXUAFIRUIRD-UHFFFAOYSA-N tripropan-2-yl stiborite Chemical compound [Sb+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] HYPTXUAFIRUIRD-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/14—Methods for preparing oxides or hydroxides in general
- C01B13/32—Methods for preparing oxides or hydroxides in general by oxidation or hydrolysis of elements or compounds in the liquid or solid state or in non-aqueous solution, e.g. sol-gel process
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
発明の目的
産業上の利用分ＩＦ
本発明は、微粉末状三酸化アンチモン−水和アルミナ複
合組成物の製造方法に関する。本発明による微粉末状三
酸化アンチモン−水和アルミナ複合組成物は各種合成樹
脂の難燃剤等の合成樹脂用添加剤あるいは顔料として用
いられる。DETAILED DESCRIPTION OF THE INVENTION OBJECTS OF THE INVENTION INDUSTRIAL APPLICATION IF The present invention relates to a method for producing a finely powdered antimony trioxide-hydrated alumina composite composition. The finely powdered antimony trioxide-hydrated alumina composite composition according to the present invention is used as an additive for synthetic resins such as a flame retardant for various synthetic resins, or as a pigment.
従来技術
従来三酸化アンチモンは乾式法で硫化アンチモンあるい
は金属アンチモンを酸化処理する等の方法で製造されて
おり、水和アルミナは湿式法でボーキサイトを力性ソー
ダ溶液で溶かしてアルミン酸ソーダとし、アルミン酸ソ
ーダ水溶液に炭酸ガスを通す等の方法で製造されていた
。Conventional technology Conventionally, antimony trioxide is produced by a dry method such as oxidizing antimony sulfide or metal antimony, and hydrated alumina is produced by a wet method by dissolving bauxite in a sodium hydroxide solution to form sodium aluminate. It was manufactured by passing carbon dioxide gas through an aqueous acid soda solution.
発明が解決しようとする問題点
従来法による三酸化アンチモンは難燃剤の用途において
平均粒径０．３〜３μと光波長領域に近く、優れた難燃
効果を示す反面隠蔽力が強く透明性を必要とする製品に
用いると白濁不透明となるという欠点があり、また、高
い難燃効果の反面、実際の火災燃焼に際しての発煙性に
ついて効果が薄いという欠点があった。Problems to be Solved by the Invention Antimony trioxide produced by the conventional method has an average particle size of 0.3 to 3μ, which is close to the wavelength range of light, and exhibits excellent flame retardant effects when used as a flame retardant. It has the disadvantage that it becomes cloudy and opaque when used in a product that requires it, and while it has a high flame retardant effect, it has a disadvantage that it has little effect on smoke generation during actual combustion.
また、水和アルミナは難燃剤の用途において透明性を有
し、有毒ガスを発生しないこと、低発煙性効果を有する
という優れた効果を持つ反面、難燃性を付与するために
多量の添加量を必要とするため、機械的特性、成形加工
性および電気的特性を低下させるという問題を有し、使
用に際しての制約が多いという欠点があった。In addition, hydrated alumina has excellent effects when used as a flame retardant in that it is transparent, does not generate toxic gas, and has a low smoke emitting effect. This has the problem of deteriorating mechanical properties, moldability, and electrical properties, and there are many restrictions on use.
発明の構成
問題点を解決するための手段
本願発明は三酸化アンチモンと水和アルミナを微粒子状
態で複合させることで、三酸化アンチモンの優れた難燃
性と水和アルミナの低発煙性と透明性を損なうことなく
両立させることを可能レニしたものであり、本願第一の
発明は（イ）アンチモン（ｍ）アルコキシドと（ロ）ア
ルミニウム（■）アルコキシドとを任意の割合で混合し
て反応させることにより複合あるいは混合アルコキシド
を作り、この反応生成物を加水分解することを特徴とす
る微粉末状三酸化アンチモン−水和アルミナ複合組成物
の製造方法に係り、本願第二の発明は（ハ）三酸化アン
チモンと（ニ）水和アルミナのいずれか一方を粉末で他
方をその成分アルコキシド（イ）または（ロ）として任
意の割合で混合して反応させ、この反応生成物を加水分
解することを特徴とする微粉末状三酸化アンチモン−水
和アルミナ複合組成物の製造方法に係る。Composition of the Invention Means for Solving Problems The present invention combines antimony trioxide and hydrated alumina in the form of fine particles, thereby achieving the excellent flame retardancy of antimony trioxide and the low smoke emission and transparency of hydrated alumina. The first invention of the present application is to mix and react (a) antimony (m) alkoxide and (b) aluminum (■) alkoxide in any ratio. The second invention of the present application relates to a method for producing a finely powdered antimony trioxide-hydrated alumina composite composition, which is characterized in that a composite or mixed alkoxide is prepared by the above reaction product, and this reaction product is hydrolyzed. It is characterized by mixing antimony oxide and (d) hydrated alumina as a powder and the other as its component alkoxide (a) or (b) in any proportion and reacting, and then hydrolyzing this reaction product. The present invention relates to a method for producing a finely powdered antimony trioxide-hydrated alumina composite composition.
本願発明においてアルコキシドとはアルコールのＯＨ基
の水素元素を金属元素アンチモンまたはアルミニウムで
置換した化合物をいう。本願発明における出発物質とし
てのアンチモン化合物には塩化物などのハロゲン化合物
があり、アルミニウム（ＩＩＩ）アルコキシドの出発物
質としては金属アルミニウムが使用される。アルコキシ
ドを作るアルコールとしてはメタノール、エタノール、
インプロパツールおよびターシャリ−ブタノール等が用
いられる。In the present invention, an alkoxide refers to a compound in which the hydrogen element of the OH group of an alcohol is replaced with a metal element antimony or aluminum. Antimony compounds used as starting materials in the present invention include halogen compounds such as chlorides, and metallic aluminum is used as a starting material for aluminum (III) alkoxide. Alcohols that make alkoxides include methanol, ethanol,
Improper tool and tertiary butanol are used.
アンチモン（ｍ）アルコキシドの調製は、アンモニア法
あるいはナトリウム法等のアルカリ金属のアルコキシド
と他方金属化合物との置換反応であるナトリウム法でも
可能である。また、アルミニウム（ＩＩＩ）アルコキシ
ドの調製は塩化第二水銀等を触媒として、金属アルミニ
ウムとアルコールとの直接反応により調製される。Antimony (m) alkoxide can also be prepared by an ammonia method or a sodium method, which is a substitution reaction of an alkali metal alkoxide with another metal compound, such as the sodium method. Further, aluminum (III) alkoxide is prepared by direct reaction of metallic aluminum and alcohol using mercuric chloride or the like as a catalyst.
アルコキシドの混合および反応は有機溶媒中で行うこと
が好ましい。これは混合の便宜を図り、反応を促進させ
るとともに後述の加水分解により生じる沈殿物の組成を
アルコキシド混合組成に一致させるためである。この有
機溶媒としてはベンゼン、トルエン、キシレンおよび前
述のアルコールが適当である。The mixing and reaction of alkoxides is preferably carried out in an organic solvent. This is for the purpose of facilitating mixing, promoting the reaction, and matching the composition of the precipitate produced by hydrolysis, which will be described later, to the alkoxide mixture composition. Suitable organic solvents are benzene, toluene, xylene and the alcohols mentioned above.
作用
本願発明は三酸化アンチモンと水和アルミナを微粒子状
態で複合させることで、三酸化アンチモンの優れた難燃
性と水和アルミナの低発煙性と透明性を損なうことなく
両立させることを可能にしたものであり、液相における
低温反応によって大掛かりな反応装置を要せずに微粉末
状三酸化アンチモン−水和アルミナ複合組成物を得るも
のである。反応温度はアンチモン（Ｉｌｌ）アルコキシ
ドおよびアルミニウム（ＩＩＩ）アルコキシドが分解す
る温度未満であれば差し支えないが、取扱いの便宜上Ｏ
〜１３０℃が望ましい。上記混合および反応による反応
生成物の加水分解は、反応溶液中に脱炭酸した蒸留水を
直接加えることにより行うことができる。この加水分解
のための反応温度はアルコキシドの調製時開様アルコキ
シドが分解せず、しかも取扱いの容易な０〜１３０℃の
範囲が適当である。この加水分解により粉末状の沈殿物
が生成する。この沈殿物を遠心分離機等により加水分解
液から分離し、必要により真空乾燥等の乾燥を行うか、
あるいは沈殿物生成溶液のスラリー濃度を調整視てスプ
レィドライにより乾燥し、必要により再乾燥等を行えば
粉末状の三酸化アンチモン−水和アルミナ複合組成物が
得られる。本願発明に使用する三酸化アンチモンおよび
水和アルミナ粉末は、アルコキシド溶液との混和性およ
び相溶性あるいは得られる複合組成物の難燃性および発
煙性をも加味して１粒径３μ以下でできるだけ細かいも
のが望ましい。Function: By combining antimony trioxide and hydrated alumina in the form of fine particles, the present invention makes it possible to achieve both the excellent flame retardancy of antimony trioxide and the low smoke emission properties of hydrated alumina without impairing transparency. A finely powdered antimony trioxide-hydrated alumina composite composition can be obtained by low-temperature reaction in a liquid phase without requiring a large-scale reaction apparatus. The reaction temperature may be lower than the temperature at which antimony (Ill) alkoxide and aluminum (III) alkoxide decompose; however, for convenience of handling, O
~130°C is desirable. Hydrolysis of the reaction product from the above mixing and reaction can be carried out by directly adding decarboxylated distilled water to the reaction solution. The reaction temperature for this hydrolysis is suitably within the range of 0 to 130 DEG C. so that the alkoxide is not decomposed during the preparation of the alkoxide and is easy to handle. This hydrolysis produces a powdery precipitate. Separate this precipitate from the hydrolyzate using a centrifuge or the like, and if necessary, dry it by vacuum drying or the like.
Alternatively, a powdered antimony trioxide-hydrated alumina composite composition can be obtained by drying by spray drying while adjusting the slurry concentration of the precipitate-forming solution and, if necessary, performing re-drying. The antimony trioxide and hydrated alumina powder used in the present invention should be as fine as possible with a particle size of 3 μm or less, taking into account the miscibility and compatibility with the alkoxide solution and the flame retardancy and smoke generation properties of the resulting composite composition. Something is desirable.
実施例 本願発明を実施例によりさらに詳しく説明する。Example The present invention will be explained in more detail with reference to Examples.
これら実施例はなんら本願発明の技術的範囲を限定する
ものではない。These Examples do not limit the technical scope of the present invention in any way.
実施例１〜３
アンチモン（ＩＩＩ）イソプロポキシドＳｂ （ｉｏＰ
ｒ）、とアルミニウム（Ｉｎ）イソプロポキシドＡｌ
（ｉｏＰｒ） ］の２種のアルコキシドを種々の組成比
で混合し、ベンゼン溶媒とともに８０℃で還流しながら
反応させた。この反応生成物に脱炭酸した蒸留水を反応
理論量の１０倍量加えて６０〜８０℃で加水分解したと
ころ、粉状の沈殿物が生成した。この沈殿物を遠心分離
により加水分解液から分離洗浄した後、７０℃で一昼夜
乾燥して粉体を得た。Examples 1-3 Antimony (III) isopropoxide Sb (ioP
r), and aluminum (In) isopropoxide Al
(ioPr)] were mixed at various composition ratios and reacted together with a benzene solvent under reflux at 80°C. When decarboxylated distilled water was added to this reaction product in an amount 10 times the theoretical reaction amount and hydrolyzed at 60 to 80°C, a powdery precipitate was generated. This precipitate was separated and washed from the hydrolysis solution by centrifugation, and then dried at 70°C for a day and night to obtain a powder.
実施例４〜５
市販の三酸化アンチモンとアルミニウムイソプロポキシ
ドとを種々の組成比で混合し、トルエン溶媒と共に１０
０〜】−１０℃で還流しながら反応させた。この反応生
成物に脱炭酸した蒸留水を大過剰加えて９０〜１１０℃
で加水分解したところ、粉状の沈殿物が生成した。この
沈殿物を遠心分離により加水分解液から分離洗浄した後
、７０℃で一昼夜乾燥して粉体を得た。Examples 4-5 Commercially available antimony trioxide and aluminum isopropoxide were mixed at various composition ratios, and 10% of the mixture was mixed with toluene solvent.
0~] The reaction was carried out under reflux at -10°C. Add a large excess of decarboxylated distilled water to this reaction product and heat to 90-111°C.
Upon hydrolysis, a powdery precipitate was formed. This precipitate was separated and washed from the hydrolysis solution by centrifugation, and then dried at 70°C for a day and night to obtain a powder.
実施例６〜７
市販の水和アルミナとアンチモン（ｍ）エトキシドＳｂ
（ＯＥｔ） 、とを種々の組成比で混合してトルエン
溶媒と共に１００〜１１０還流しながら反応させた９こ
の反応生成物に脱炭酸したエタノール水溶液を反応理論
量の１０倍量加えて９０〜１１０℃で加水分解したとこ
ろ、粉状の沈殿物が生成した。この沈殿物を遠心分離に
より加水分解液から分離洗浄した後、７０℃で一昼夜乾
燥して粉体を得た。Examples 6-7 Commercially available hydrated alumina and antimony (m) ethoxide Sb
(OEt) in various composition ratios and reacted with a toluene solvent while refluxing at 100-110°C. 9 To this reaction product, a decarboxylated ethanol aqueous solution was added in an amount 10 times the theoretical reaction amount to give a reaction product of 90-110°C. Hydrolysis at °C produced a powdery precipitate. This precipitate was separated and washed from the hydrolysis solution by centrifugation, and then dried at 70°C for a day and night to obtain a powder.
上記の各実施例で得られた粉体を用いた各種組成物をロ
ールで混練後加熱プレスでシートを作成した。作成した
シートについて各種物性を測定した結果を当該粉体の三
酸化アンチモン、水和アルミナ組成とともに第−表に示
す。Various compositions using the powder obtained in each of the above Examples were kneaded with a roll and then heated to form a sheet. The results of measuring various physical properties of the prepared sheet are shown in Table 1 along with the antimony trioxide and hydrated alumina composition of the powder.
また、日本精鉱株式会社製三酸化アンチモン（平均粒径
０．６μ）および昭和軽金属株式会社製氷和アルミナ（
平均粒径１．０μ）を用いた組成物およびこれらのいず
れをも用いない組成物をロールで混練後加熱プレスでシ
ートを作成し、これらシートについて各種物性を測定し
た結果を第二人に示す。In addition, antimony trioxide (average particle size 0.6μ) manufactured by Nippon Seiko Co., Ltd. and Hyowa alumina (manufactured by Showa Light Metal Co., Ltd.)
After kneading a composition using a mean particle size of 1.0μ) and a composition using neither of these using a roll, sheets were created using a hot press, and the results of measuring various physical properties of these sheets were shown to a second person. .
これら２表の測定結果に示されるように、本願発明の粉
体を用いた場合、従来の三酸化アンチモンを用いる場合
に比べて、三酸化アンチモン過剰から水和アルミナ半量
程度までは同程度の難燃効果を有し、加えて透明性に優
れた結果を示し、従来の水和アルミナを用いる場合に比
べて透明性をあまり低下せずに難燃効果が期待できる結
果となった・
第 −表
第 二 表
（注）
（１）酸素指数：ＪＩＳ Ｋ ７２０１ による側定値
（２）透明性 ：表記載組成シートのカラーメーターに
よる光透過率り値
発明の効果
本願発明によれば、高純度の超微粒子が得られるアルコ
キシド法の特徴を生かして、アンチモン（ＩＩＩ）アル
コキシドおよびアルミニウム（ＩＩＩ）アルコキシドの
いずれか一方をその成分粉末で使用するか、両方をアル
コキシドで使用することにより、各組成比を目的に応す
る割合に任意に混合する反応と、その加水分解反応とに
より目的組成の微粉末状三酸化アンチモン−水和アルミ
ナ複合組成物を得ることができる。この複合組成物粉末
は。As shown in the measurement results in these two tables, when the powder of the present invention is used, compared to the case where conventional antimony trioxide is used, from an excess of antimony trioxide to about half the amount of hydrated alumina, the difficulty is the same. It has a flame retardant effect and also shows excellent transparency, and compared to the case of using conventional hydrated alumina, the flame retardant effect can be expected without much reduction in transparency. Table 2 (Note) (1) Oxygen index: Determined value according to JIS K 7201 (2) Transparency: Light transmittance value measured by a color meter of the composition sheet listed in the table Effect of the invention According to the present invention, high purity ultra Taking advantage of the characteristics of the alkoxide method that yields fine particles, each composition ratio can be adjusted to the desired composition by using either antimony (III) alkoxide or aluminum (III) alkoxide in its component powder, or by using both in their alkoxide form. A finely powdered antimony trioxide-hydrated alumina composite composition having the desired composition can be obtained by a reaction in which the antimony trioxide and hydrated alumina composite composition is arbitrarily mixed in a proportion corresponding to the desired composition and a hydrolysis reaction thereof. This composite composition powder.
難燃性、透明性および低発煙性に優れた高機能這燃剤、
あるいは顔料として有効利用が期待できるものである。A high-performance flame retardant with excellent flame retardancy, transparency, and low smoke emission.
Alternatively, it can be expected to be effectively used as a pigment.
Claims (2)
アルミニウム（III）アルコキシドとを任意の割合で混
合して反応させることにより複合あるいは混合アルコキ
シドを作り、この反応生成物を加水分解することを特徴
とする微粉末状三酸化アンチモン−水和アルミナ複合組
成物の製造方法(1) (a) antimony (III) alkoxide and (b)
A finely powdered antimony trioxide-hydrated alumina composite composition characterized in that a composite or mixed alkoxide is produced by mixing and reacting with aluminum (III) alkoxide in an arbitrary ratio, and this reaction product is hydrolyzed. method of manufacturing things
いずれか一方を粉末で他方をその成分アルコキシド（イ
）または（ロ）として任意の割合で混合して反応させ、
この反応生成物を加水分解することを特徴とする微粉末
状三酸化アンチモン−水和アルミナ複合組成物の製造方
法(2) (c) Antimony trioxide and (d) hydrated alumina are mixed as a powder and the other as its component alkoxide (a) or (b) in an arbitrary ratio and reacted;
A method for producing a finely powdered antimony trioxide-hydrated alumina composite composition, which comprises hydrolyzing this reaction product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19043486A JPS6350321A (en) | 1986-08-15 | 1986-08-15 | Production of fine-powdery antimony trioxide-hydrated alumina composite composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19043486A JPS6350321A (en) | 1986-08-15 | 1986-08-15 | Production of fine-powdery antimony trioxide-hydrated alumina composite composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS6350321A true JPS6350321A (en) | 1988-03-03 |
Family
ID=16258066
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19043486A Pending JPS6350321A (en) | 1986-08-15 | 1986-08-15 | Production of fine-powdery antimony trioxide-hydrated alumina composite composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6350321A (en) |
-
1986
- 1986-08-15 JP JP19043486A patent/JPS6350321A/en active Pending
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