JPH03285824A - Superfine-grain antimony pentoxide surface-treated with fluorine-containing silane compound and its production - Google Patents
Superfine-grain antimony pentoxide surface-treated with fluorine-containing silane compound and its productionInfo
- Publication number
- JPH03285824A JPH03285824A JP8398290A JP8398290A JPH03285824A JP H03285824 A JPH03285824 A JP H03285824A JP 8398290 A JP8398290 A JP 8398290A JP 8398290 A JP8398290 A JP 8398290A JP H03285824 A JPH03285824 A JP H03285824A
- Authority
- JP
- Japan
- Prior art keywords
- antimony pentoxide
- fluorine
- hydrochloric acid
- pts
- sodium antimonate
- 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
- LJCFOYOSGPHIOO-UHFFFAOYSA-N antimony pentoxide Chemical compound O=[Sb](=O)O[Sb](=O)=O LJCFOYOSGPHIOO-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 12
- 229910052731 fluorine Inorganic materials 0.000 title claims description 13
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims description 11
- 239000011737 fluorine Substances 0.000 title claims description 11
- -1 silane compound Chemical class 0.000 title claims description 11
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 50
- NSBGJRFJIJFMGW-UHFFFAOYSA-N trisodium;stiborate Chemical compound [Na+].[Na+].[Na+].[O-][Sb]([O-])([O-])=O NSBGJRFJIJFMGW-UHFFFAOYSA-N 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 4
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 13
- 239000000758 substrate Substances 0.000 claims 1
- 239000011347 resin Substances 0.000 abstract description 12
- 229920005989 resin Polymers 0.000 abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000047 product Substances 0.000 abstract description 5
- 239000002244 precipitate Substances 0.000 abstract description 3
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 abstract description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 20
- 239000003063 flame retardant Substances 0.000 description 8
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- 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 6
- 238000003756 stirring Methods 0.000 description 6
- 238000002834 transmittance Methods 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 5
- 229910052787 antimony Inorganic materials 0.000 description 4
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 238000004381 surface treatment Methods 0.000 description 4
- QEZIKGQWAWNWIR-UHFFFAOYSA-N antimony(3+) antimony(5+) oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[Sb+3].[Sb+5] QEZIKGQWAWNWIR-UHFFFAOYSA-N 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 150000004687 hexahydrates Chemical class 0.000 description 3
- 239000011164 primary particle Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000011368 organic material Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- AQTIRDJOWSATJB-UHFFFAOYSA-K antimonic acid Chemical compound O[Sb](O)(O)=O AQTIRDJOWSATJB-UHFFFAOYSA-K 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- DAMJCWMGELCIMI-UHFFFAOYSA-N benzyl n-(2-oxopyrrolidin-3-yl)carbamate Chemical compound C=1C=CC=CC=1COC(=O)NC1CCNC1=O DAMJCWMGELCIMI-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 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
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000007863 gel particle Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、分散性に優れた平均粒子径０．１μｍ以下の
超微粒子五酸化アンチモンおよびその製造方法に関する
ものであり、この粉末を分散させた成形膜および成形体
は優れた透明性と難燃効果を有する。Detailed Description of the Invention [Field of Industrial Application] The present invention relates to ultrafine antimony pentoxide particles having an average particle diameter of 0.1 μm or less and excellent dispersibility, and a method for producing the same. The molded film and molded body have excellent transparency and flame retardant effect.
近年、有機材料がいたるところで使用されており、プラ
スチックをはじめ、はとんどの有機材料が可燃性であり
大気中で容易に燃焼し、火災の際初期段階で着火し、煙
、有毒ガスを発生する。従って、火災の初期段階の３０
０〜５００℃で燃えにくくするために難燃剤を添加し、
難燃化機能をもたせている。特に自動車や電子機器など
に用いられる材料は難燃化されていないと使用すること
ができない箇所もあり、難燃化は非常に重要となる。ア
ンチモン系難燃剤はハロゲンと組み合わせることにより
優れた難燃効果をだすことができる。本発明品は、超微
粒子であるため光の散乱を小さくすることができ、光の
透過性が高められるので透明性プラスチックスおよび透
明性フィルムの難燃性フィラーとして利用することが出
来る。In recent years, organic materials have become ubiquitous, and most organic materials, including plastics, are flammable and easily burn in the atmosphere, igniting in the early stages of a fire, producing smoke and toxic gases. do. Therefore, in the early stages of a fire, 30
Flame retardants are added to make it less flammable at temperatures between 0 and 500 degrees Celsius.
It has a flame retardant function. In particular, flame retardancy is extremely important, as there are some parts of materials used in automobiles and electronic devices that cannot be used unless they are flame retardant. Antimony-based flame retardants can exhibit excellent flame retardant effects when combined with halogens. Since the product of the present invention is an ultrafine particle, light scattering can be reduced and light transmittance is increased, so it can be used as a flame-retardant filler for transparent plastics and transparent films.
アンチモン系難燃剤のなかで二酸化アンチモンは優れた
難燃剤として多量に使用されているが、毒性が強く規制
される傾向にあり、毒性の弱い五酸化アンチモンへの代
替を検討する必要がでてきた。また最近プラスチックス
あるいはフィルムに透明性を付与して機能を高めること
が望まれており、粉末の微粒子化が要求されている。Among antimony-based flame retardants, antimony dioxide is widely used as an excellent flame retardant, but its toxicity tends to be heavily regulated, making it necessary to consider replacing it with antimony pentoxide, which is less toxic. . Recently, it has been desired to improve the functionality of plastics or films by imparting transparency, and there is a demand for finer particles of powder.
五酸化アンチモンの一般的な製法として、アンチモン酸
アルカリの脱イオンおよび酸分解によって得る方法と三
塩化アンチモンの加水分解物或は二酸化アンチモンの酸
化による方法がある。これら湿式法によって得られる五
酸化アンチモンは微細なゲルあるいはゾルで、これより
得られる粉末は粒子径が０．１μｍ以下であり、二酸化
アンチモンに比べて容易に微粒子化ができる。しかし−
船釣に、湿式法によって得られる五酸化アンチモンは結
晶性の高い微細なゲル粒子であり、酸性度が低下すると
ともに解膠して安定なゾルを形成する。Common methods for producing antimony pentoxide include a method in which it is obtained by deionization and acid decomposition of alkali antimonate, and a method in which it is obtained by oxidation of a hydrolyzate of antimony trichloride or antimony dioxide. Antimony pentoxide obtained by these wet methods is a fine gel or sol, and the powder obtained therefrom has a particle size of 0.1 μm or less, and can be more easily made into fine particles than antimony dioxide. But-
Antimony pentoxide, which is obtained by a wet method for boat fishing, is a highly crystalline fine gel particle that peptizes as the acidity decreases to form a stable sol.
しかもゾルを生成すると粉末化することが困難で乾燥時
に凝集し分散性の良い粉末を得ることができない。従っ
て安定なアンチモンゾルとして使用するか、あるいは粉
末の表面処理を行って分散性を高めることがなされてい
るが、粉末については必ずしも十分な効果を挙げていな
い。Moreover, once a sol is produced, it is difficult to powder it, and it aggregates during drying, making it impossible to obtain a powder with good dispersibility. Therefore, efforts have been made to improve dispersibility by using antimony as a stable antimony sol or by surface treating the powder, but these efforts have not always produced sufficient effects for the powder.
本発明者は分散性に優れた超微粒子五酸化アンチモン粉
末について鋭意検討した結果、アンチモン酸ナトリウム
を塩酸に溶解抜水に滴下することによって超微粒子五酸
化アンチモンを生成し、その後含フッ素シラン化合物で
表面処理を行なう手法を見出した。As a result of intensive studies on ultrafine antimony pentoxide powder with excellent dispersibility, the inventors produced ultrafine antimony pentoxide by dissolving sodium antimonate in hydrochloric acid and dropping it into drained water, and then adding it to a fluorine-containing silane compound. We have discovered a method for surface treatment.
本発明は、一般式Ｃ，Ｆｌ、 ５Ｏ２ＮＲＣＨ２ＣＨ２
ＣＨ２ＳｉＸ、 テ表され１式中ＲはＣ１−５のアルキ
ル基、ＸはＣｌ、Ｂｒ、ＯＣＨ３、ＱＣ，）ｌｓである
含フッ素シラン化合物が表面に基質１００重量部に対し
て０．０１〜５．０重量部の割で付着結合していること
を特徴とする平均粒子径０．１μｍ以下の分散性に優れ
た超微粒子五酸化アンチモンを提供する。The present invention has the general formula C, Fl, 5O2NRCH2CH2
CH2SiX, represented by formula 1, where R is a C1-5 alkyl group and X is Cl, Br, OCH3, QC, The present invention provides ultrafine antimony pentoxide particles having an average particle diameter of 0.1 μm or less and having excellent dispersibility, which are adhesively bonded at a proportion of .0 parts by weight.
本発明はまたアンチモン酸ナトリウムを塩酸で溶解後、
アンチモン酸ナトリウム塩酸溶液を水に滴下して五酸化
アンチモンを生成し、その後で含フッ素シラン化合物で
表面処理することを特徴とする上記の平均粒子径０．１
μｍ以下の分散性に優れた超微粒子五酸化アンチモンの
製造方法を提供する。The present invention also provides that after dissolving sodium antimonate with hydrochloric acid,
The above average particle diameter of 0.1 is characterized in that antimony pentoxide is produced by dropping a sodium antimonate hydrochloric acid solution into water, and then the surface is treated with a fluorine-containing silane compound.
Provided is a method for producing ultrafine antimony pentoxide particles with excellent dispersibility of micrometers or less.
本発明の方法において、アンチモン酸ナトリウム塩酸溶
液は好ましくはアンチモン酸ナトリウム１００重量部を
塩酸１３０〜２７０重量部に溶解して調製する。さらに
アンチモン酸ナトリウムの溶解性を高めるためにアンチ
モン酸ナトリウム塩酸溶液を６０℃以上に加温すること
が好ましい。塩酸が１３０重量部以下ではアンチモン酸
ナトリウムの溶解が不十分でペースト状になりやすく、
塩酸が２７０重量部以上ではアンチモン酸ナトリウム塩
酸溶液中にアンチモン酸ゲル或は塩化ナトリウムを析出
しやすく、さらに水に滴下した際、酸濃度が高く五酸化
アンチモンが比較的に生成しにくい。本発明に用いられ
るアンチモン酸ナトリウムは一般的な六水塩のものが使
用されるが結晶水の少ないものでもよい。In the method of the invention, the sodium antimonate hydrochloric acid solution is preferably prepared by dissolving 100 parts by weight of sodium antimonate in 130 to 270 parts by weight of hydrochloric acid. Further, in order to increase the solubility of sodium antimonate, it is preferable to heat the sodium antimonate hydrochloric acid solution to 60° C. or higher. When hydrochloric acid is less than 130 parts by weight, sodium antimonate is not sufficiently dissolved and tends to become paste-like.
When the amount of hydrochloric acid is 270 parts by weight or more, antimonic acid gel or sodium chloride tends to precipitate in the sodium antimonate hydrochloric acid solution, and furthermore, when the solution is dropped into water, the acid concentration is high and antimony pentoxide is relatively difficult to form. As the sodium antimonate used in the present invention, a general hexahydrate salt is used, but a sodium antimonate with less crystallization water may be used.
上記アンチモン酸ナトリウム塩酸溶液を水に滴下する際
、アンチモン酸ナトリウム塩酸溶液１００重量部に対し
て３００重量部以上の水を用いるのが好ましい。さらに
、生成ゲルの凝集を防止するため、アンチモン酸ナトリ
ウム塩酸溶液は６０℃以上に加温して攪拌されている水
に滴下するのが好ましい。水が３００重量部以下では生
成した水和五酸化アンチモンゲルの分散がよくなく、含
フッ素シラン化合物による表面処理を十分に行なうこと
ができず分散性が低下する。When the sodium antimonate hydrochloric acid solution is added dropwise to water, it is preferable to use 300 parts by weight or more of water per 100 parts by weight of the sodium antimonate hydrochloric acid solution. Furthermore, in order to prevent agglomeration of the produced gel, it is preferable that the sodium antimonate hydrochloric acid solution be dropped into water that has been heated to 60° C. or higher and stirred. If the amount of water is less than 300 parts by weight, the produced hydrated antimony pentoxide gel will not be well dispersed, and the surface treatment with the fluorine-containing silane compound will not be able to be carried out sufficiently, resulting in a decrease in dispersibility.
含フッ素シラン化合物による表面処理は上記水和五酸化
アンチモンゲルを脱水後、アルコール１００重量部に五
酸化アンチモンを３０重量部分散させた後、五酸化アン
チモン１００重量部に対して含フッ素シラン化合物を０
．０１〜５．０重量部添加して表面処理を行なう。この
範囲外において、含フッ素シラン化合物が０．０１重量
部未満では五酸化アンチモンを樹脂に分散させた際、十
分な分散効果が現われず、５．０重量部を超えると粉末
の撥水性、撥油性が現われ樹脂に分散しにくくなる。Surface treatment with a fluorine-containing silane compound is carried out by dehydrating the hydrated antimony pentoxide gel, dispersing 30 parts by weight of antimony pentoxide in 100 parts by weight of alcohol, and then applying a fluorine-containing silane compound to 100 parts by weight of antimony pentoxide. 0
．． Surface treatment is performed by adding 01 to 5.0 parts by weight. Outside this range, if the fluorine-containing silane compound is less than 0.01 part by weight, a sufficient dispersion effect will not be obtained when antimony pentoxide is dispersed in a resin, and if it exceeds 5.0 parts by weight, the water repellency of the powder will decrease. It becomes oily and becomes difficult to disperse into the resin.
本発明に用いられる含フッ素シラン化合物は、−船釣Ｃ
５Ｆ１．５ｏ２ＮＲＣＨ２Ｃ）１２ ＣＨ２５ｉＸ３
（式中ＲはＣＸ−５のアルキル基、ＸはＣ１、Ｂｒ、Ｏ
ＣＨ，、ＱＣ２Ｈ，）で表され、これらのうち何れを用
いても良い。これらの化合物は特願昭６３−１０１４６
３号公報に記載されている。The fluorine-containing silane compound used in the present invention is - Funatsuri C
5F1.5o2NRCH2C)12 CH25iX3
(In the formula, R is an alkyl group of CX-5, X is C1, Br, O
CH,,QC2H,), and any of these may be used. These compounds are disclosed in Japanese Patent Application No. 63-10146.
It is described in Publication No. 3.
以下に実施例により本発明を具体的に説明する。 The present invention will be specifically explained below using Examples.
実施例１
アンチモン酸ナトリウム（六水塩）５０ｇを試薬特級塩
酸（３６％）６５ｇに攪拌しながら少量ずつ滴下した後
６０℃に加温し、アンチモン酸ナトリウム塩酸溶液を調
製した。このアンチモン酸ナトリウム塩酸溶液を６０℃
に加温してイオン交換水４００ｇに１０分かけて滴下し
５０℃で２時間攪拌した後生成物を沈殿させた。その後
、沈殿物を濾過し濾液の抵抗値が３０００Ω以上になる
まで沈殿物を洗浄し、脱水した。次に脱水した粉末をエ
チルアルコール１００ｇに分散させた後、含フッ素シラ
ン化合物としてＣ，Ｆ□７Ｓｏ２Ｎ （Ｃ３Ｈ，）ＣＨ
２ＣＨ２ＣＨ２Ｓｉ （ｏｃｚ ｕ、 ）３ （”ＭＦ
−１６０”、三菱金属（株）製）を１％溶解したエチル
アルコール溶液０．３ｇを添加して１０時間室温で攪拌
し、濾過乾燥後粉砕した。ここで得られた粉末の比表面
積は３８ｒｎ’／ｇで一次粒子径は０．０４３μｍであ
った。この粉末０．５ｇを塩化ビニル樹脂５０ｇにヒー
トロールを用いて１３０℃で練り込み０．３ｍｍにプレ
スした後、可視紫外分光光度計で透過率を測定した。そ
の結果を第１図に示した。波長６００ｎｍにおいて粉末
無添加の塩化ビニル樹脂に対して６５％の透明性を維持
した。Example 1 50 g of sodium antimonate (hexahydrate) was added dropwise little by little to 65 g of reagent grade hydrochloric acid (36%) with stirring, and then heated to 60° C. to prepare a sodium antimonate hydrochloric acid solution. This sodium antimonate hydrochloric acid solution was heated at 60°C.
The mixture was added dropwise to 400 g of ion-exchanged water over 10 minutes, and the mixture was stirred at 50° C. for 2 hours to precipitate the product. Thereafter, the precipitate was filtered, washed until the resistance value of the filtrate became 3000Ω or more, and dehydrated. Next, after dispersing the dehydrated powder in 100 g of ethyl alcohol, C,F□7So2N (C3H,)CH
2CH2CH2Si (ocz u, )3 (”MF
0.3 g of an ethyl alcohol solution containing 1% of ``-160'' (manufactured by Mitsubishi Metals Co., Ltd.) was added, stirred at room temperature for 10 hours, filtered and dried, and then ground.The specific surface area of the powder obtained here was 38rn. '/g, and the primary particle size was 0.043 μm. 0.5 g of this powder was kneaded into 50 g of vinyl chloride resin at 130°C using a heat roll, pressed to 0.3 mm, and then measured using a visible and ultraviolet spectrophotometer. Transmittance was measured. The results are shown in Figure 1. At a wavelength of 600 nm, 65% transparency was maintained compared to vinyl chloride resin without powder addition.
実施例２
アンチモン酸ナトリウム（六水塩）５０ｇを試薬特級塩
酸（３６％）１３５ｇに攪拌しながら少量ずつ滴下した
後６０℃に加温しアンチモン酸ナトリウム塩酸溶液を調
製した。このアンチモン酸ナトリウム塩酸溶液を６０℃
に加温して攪拌中の水１５０ｇに２０分かけて滴下し、
５０℃で２時間攪拌した後生成物を沈殿させた。次に、
脱水した粉末をエチルアルコール１００ｇに分散させた
後、含フッ素シラン化合物としてＣ，Ｆ□、 ５ｏ２Ｎ
（Ｃ３Ｈ７）ＣＨ２ＣＨ２ＣＨ２ＳｉＣΩ３（三菱金
属■製）を１０％溶解したエチルアルコール溶液１５ｇ
を添加して１０時間室温で攪拌し、濾過乾燥後粉砕した
。Example 2 50 g of sodium antimonate (hexahydrate) was added dropwise little by little to 135 g of reagent grade hydrochloric acid (36%) with stirring, and then heated to 60° C. to prepare a sodium antimonate hydrochloric acid solution. This sodium antimonate hydrochloric acid solution was heated at 60°C.
Add it dropwise over 20 minutes to 150g of water while stirring.
The product was precipitated after stirring for 2 hours at 50°C. next,
After dispersing the dehydrated powder in 100 g of ethyl alcohol, C, F□, 5o2N were added as fluorine-containing silane compounds.
15g of ethyl alcohol solution containing 10% (C3H7)CH2CH2CH2SiCΩ3 (manufactured by Mitsubishi Metals)
was added, stirred at room temperature for 10 hours, filtered and dried, and then ground.
ここで得られた粉末の比表面積は３０♂／ｇで一次粒子
径は０．０５４μｍであった。この粉末０．５ｇを塩化
ビニル樹脂５０ｇにヒートロールを用いて１３０℃で練
り込み０ 、３ｍｍにプレスした後、可視紫外分光光度
計で透過率を測定した。この粉末を実施例１と同様に塩
化ビニル樹脂に練り込みプレスした後、可視紫外分光光
度計で透過率を測定した。その結果波長６００ｎｍにお
いて無添加の塩化ビニル樹脂に対して６０％の透明性を
維持した。The powder thus obtained had a specific surface area of 30♂/g and a primary particle size of 0.054 μm. After kneading 0.5 g of this powder into 50 g of vinyl chloride resin at 130° C. using a heat roll and pressing it to a thickness of 0.3 mm, transmittance was measured using a visible and ultraviolet spectrophotometer. This powder was kneaded into vinyl chloride resin and pressed in the same manner as in Example 1, and then the transmittance was measured using a visible and ultraviolet spectrophotometer. As a result, at a wavelength of 600 nm, 60% transparency was maintained compared to additive-free vinyl chloride resin.
比較例１
アンチモン酸ナトリウム（六水塩）５０ｇを試薬特級塩
酸（３６％）６５ｇに攪拌しながら少量ずつ滴下した後
６０℃に加温しアンチモン酸ナトリウム塩酸溶液を調整
した。このアンチモン酸ナトリウム塩酸溶液を６０℃に
加温してイオン交換水４００ｇに１０分かけて滴下し５
０℃で２時間攪拌した後生成物を沈殿させた。その後、
沈殿物を濾過し濾液の抵抗値が３０００Ω以上になるま
で沈殿物を洗浄し、脱水、乾燥後粉砕した。ここで得ら
れた粉末の比表面積は３５ｒｒｆ／ｇで一次粒子径は０
．０４６μｍであった。この粉末を実施例１と同様に塩
化ビニル樹脂に練り込みプレスした後、可視紫外分光光
度計で透過率を測定した。その結果は第１図に示したよ
うに波長６００ｎｍにおいて無添加の塩化ビニル樹脂に
対して５３％の透明性であった。Comparative Example 1 50 g of sodium antimonate (hexahydrate) was added dropwise little by little to 65 g of reagent grade hydrochloric acid (36%) with stirring, and then heated to 60° C. to prepare a sodium antimonate hydrochloric acid solution. This sodium antimonate hydrochloric acid solution was heated to 60°C and added dropwise to 400 g of ion-exchanged water over 10 minutes.
The product was precipitated after stirring for 2 hours at 0°C. after that,
The precipitate was filtered, washed until the resistance value of the filtrate became 3000Ω or more, dehydrated, dried, and pulverized. The specific surface area of the powder obtained here is 35rrf/g and the primary particle size is 0.
．． It was 046 μm. This powder was kneaded into vinyl chloride resin and pressed in the same manner as in Example 1, and then the transmittance was measured using a visible and ultraviolet spectrophotometer. As shown in FIG. 1, the transparency at a wavelength of 600 nm was 53% compared to additive-free vinyl chloride resin.
以上実施例で述べたように本発明によって得られる五酸
化アンチモン粉末は樹脂に混練しても６０％以上の高い
透明性を維持し、優れた分散性を有した超微粒子五酸化
アンチモン粉末を提供することが出来る。As described in the examples above, the antimony pentoxide powder obtained by the present invention maintains a high transparency of 60% or more even when mixed with resin, and provides ultrafine antimony pentoxide powder with excellent dispersibility. You can.
従って、本発明による超微粒子五酸化アンチモンは、透
明性プラスチックス或は透明性フィルムのＪｉｌＩＭ性
フィラーとして利用することが出来る。Therefore, the ultrafine antimony pentoxide particles according to the present invention can be used as a JILIM filler for transparent plastics or transparent films.
添付第１図はプラスチックシートの各波長における光線
透過率を示すグラフである。Attached FIG. 1 is a graph showing the light transmittance of the plastic sheet at each wavelength.
Claims (1)
＿２ＣＨ＿２ＳｉＸ＿３で表され、式中ＲはＣ＿１＿−
＿５のアルキル基、ＸはＣｌ、Ｂｒ、ＯＣＨ＿３、ＯＣ
＿２Ｈ＿５である含フッ素シラン化合物が表面に基質１
００重量部に対して０．０１〜５．０重量部の割で付着
結合していることを特徴とする平均粒子径０．１μｍ以
下の分散性に優れた超微粒子五酸化アンチモン。 ２、アンチモン酸ナトリウムを塩酸で溶解後、アンチモ
ン酸ナトリウム塩酸溶液を水に滴下して五酸化アンチモ
ンを生成し、その後で含フッ素シラン化合物で表面処理
することを特徴とする特許請求の範囲１に記載の平均粒
子径０．１μｍ以下の分散性に優れた超微粒子五酸化ア
ンチモンの製造方法。[Claims] 1. General formula C_9F_1_7SO_2NRCH_2CH
It is represented by _2CH_2SiX_3, where R is C_1_-
_5 alkyl group, X is Cl, Br, OCH_3, OC
The fluorine-containing silane compound _2H_5 is placed on the surface of the substrate 1.
Ultrafine antimony pentoxide particles with an average particle diameter of 0.1 μm or less and excellent dispersibility, characterized in that 0.01 to 5.0 parts by weight of antimony pentoxide are adhesively bonded to 0.00 parts by weight. 2. Claim 1 characterized in that after dissolving sodium antimonate in hydrochloric acid, the sodium antimonate solution in hydrochloric acid is dropped into water to produce antimony pentoxide, and then the surface is treated with a fluorine-containing silane compound. A method for producing ultrafine antimony pentoxide particles having an average particle diameter of 0.1 μm or less and excellent dispersibility.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8398290A JPH03285824A (en) | 1990-03-30 | 1990-03-30 | Superfine-grain antimony pentoxide surface-treated with fluorine-containing silane compound and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8398290A JPH03285824A (en) | 1990-03-30 | 1990-03-30 | Superfine-grain antimony pentoxide surface-treated with fluorine-containing silane compound and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03285824A true JPH03285824A (en) | 1991-12-17 |
Family
ID=13817739
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8398290A Pending JPH03285824A (en) | 1990-03-30 | 1990-03-30 | Superfine-grain antimony pentoxide surface-treated with fluorine-containing silane compound and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03285824A (en) |
-
1990
- 1990-03-30 JP JP8398290A patent/JPH03285824A/en active Pending
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