JPH02194064A - Antimony-containing fine particle titanium dioxide powder - Google Patents
Antimony-containing fine particle titanium dioxide powderInfo
- Publication number
- JPH02194064A JPH02194064A JP1333989A JP1333989A JPH02194064A JP H02194064 A JPH02194064 A JP H02194064A JP 1333989 A JP1333989 A JP 1333989A JP 1333989 A JP1333989 A JP 1333989A JP H02194064 A JPH02194064 A JP H02194064A
- Authority
- JP
- Japan
- Prior art keywords
- titanium dioxide
- antimony
- fine particle
- particle
- fine
- 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
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 79
- 239000004408 titanium dioxide Substances 0.000 title claims description 35
- 239000010419 fine particle Substances 0.000 title claims description 23
- 239000000843 powder Substances 0.000 title claims description 11
- 229910052787 antimony Inorganic materials 0.000 title claims description 8
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims description 8
- 239000002245 particle Substances 0.000 claims description 19
- 229910000410 antimony oxide Inorganic materials 0.000 claims description 7
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 2
- SZOADBKOANDULT-UHFFFAOYSA-K antimonous acid Chemical compound O[Sb](O)O SZOADBKOANDULT-UHFFFAOYSA-K 0.000 claims 1
- 150000001463 antimony compounds Chemical class 0.000 claims 1
- 239000007900 aqueous suspension Substances 0.000 claims 1
- 239000011247 coating layer Substances 0.000 claims 1
- 238000010304 firing Methods 0.000 claims 1
- 230000003472 neutralizing effect Effects 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 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 6
- 239000003063 flame retardant Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 229920000915 polyvinyl chloride Polymers 0.000 description 5
- 239000004800 polyvinyl chloride Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000049 pigment Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 239000000976 ink Substances 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical class [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- YNLFZBFVJFNCSG-UHFFFAOYSA-K Cl.[Sb](Cl)(Cl)Cl Chemical compound Cl.[Sb](Cl)(Cl)Cl YNLFZBFVJFNCSG-UHFFFAOYSA-K 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- AZTSDLGKGCQZQJ-UHFFFAOYSA-N antimony;hydrate Chemical compound O.[Sb] AZTSDLGKGCQZQJ-UHFFFAOYSA-N 0.000 description 1
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 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
- GWOWVOYJLHSRJJ-UHFFFAOYSA-L cadmium stearate Chemical compound [Cd+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O GWOWVOYJLHSRJJ-UHFFFAOYSA-L 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- OCWMFVJKFWXKNZ-UHFFFAOYSA-L lead(2+);oxygen(2-);sulfate Chemical compound [O-2].[O-2].[O-2].[Pb+2].[Pb+2].[Pb+2].[Pb+2].[O-]S([O-])(=O)=O OCWMFVJKFWXKNZ-UHFFFAOYSA-L 0.000 description 1
- UMKARVFXJJITLN-UHFFFAOYSA-N lead;phosphorous acid Chemical compound [Pb].OP(O)O UMKARVFXJJITLN-UHFFFAOYSA-N 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- SJOCPYUKFOTDAN-ZSOIEALJSA-N methyl (4z)-4-hydroxyimino-6,6-dimethyl-3-methylsulfanyl-5,7-dihydro-2-benzothiophene-1-carboxylate Chemical compound C1C(C)(C)C\C(=N\O)C=2C1=C(C(=O)OC)SC=2SC SJOCPYUKFOTDAN-ZSOIEALJSA-N 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
- 230000000737 periodic effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/36—Compounds of titanium
- C09C1/3607—Titanium dioxide
- C09C1/3653—Treatment with inorganic compounds
- C09C1/3661—Coating
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
本発明は、粒子表面及び／又は粒子内部にアンチモン酸
化物を存在させた微粒子二酸化チタン粉末で、その大き
さが０．１μ以下であり、アンチモン酸化物の量がｓｂ
！ｏ、として０．１〜５０％含有する微粉末に関する。Detailed Description of the Invention The present invention provides fine particle titanium dioxide powder in which antimony oxide is present on the particle surface and/or inside the particle, the size of which is 0.1μ or less, and the amount of antimony oxide is sb.
! It relates to a fine powder containing 0.1 to 50% as o.
この微粒子二酸化チタン粉末は、塗料、インキ、あるい
はプラスチックスに配合された時、光に対して非常に安
定でかつ透明であり、紫外線遮蔽性を有し、更に難燃化
を有する。When this fine particle titanium dioxide powder is incorporated into paints, inks, or plastics, it is very stable and transparent to light, has ultraviolet shielding properties, and has flame retardant properties.
一般に、微粒子二酸化チタン粉末は、０．１〜０゜４μ
の大きさを有する顔料用酸化チタンに比べ、異なる挙動
を示すことはよく知られている。Generally, fine particle titanium dioxide powder is 0.1~0°4μ
It is well known that titanium oxide exhibits different behavior compared to titanium oxide for pigments, which has a size of .
例えば、プラスチックスに配合された場合、その粒子径
が極めて小さい為、透明かつ紫外線遮蔽剤の機能を有す
る。For example, when incorporated into plastics, the particle size is extremely small, so it is transparent and has the function of an ultraviolet shielding agent.
しかしながら、光特に紫外線が照射されることにより、
プラスチックスの主体である樹脂の劣化をも早めたり、
あるいは樹脂の変色を生じることとなる。However, when exposed to light, especially ultraviolet light,
It also accelerates the deterioration of resin, which is the main component of plastics,
Alternatively, discoloration of the resin may occur.
このような現象の理論は、充分解明されていないが、こ
のような欠点を防ぐ為に特開昭６３−４５１２３には、
０．０１〜０．１μの範囲内の大きさのものが８０％以
上であるような微粒子の二酸化チタン粉末に、ケイ素及
び／又はアルミニウムの酸化物を被覆したものが提案さ
れている。Although the theory behind this phenomenon has not been fully elucidated, in order to prevent this drawback, Japanese Patent Application Laid-Open No. 63-45123
It has been proposed that fine particles of titanium dioxide powder, 80% or more of which have a size within the range of 0.01 to 0.1 microns, are coated with silicon and/or aluminum oxides.
このようなケイ素及び／又はアルミニウムの酸化物の被
覆は、光に対して安定化を高める効果があるものの、二
酸化チタンの木質的な改良になっていない為に被覆を行
っているにもかかわらず、そのものの光に対する安定性
はもう一歩である。Although such silicon and/or aluminum oxide coatings have the effect of increasing stabilization against light, they do not improve the wood quality of titanium dioxide. , its stability against light is another step forward.
微粒子二酸化チタンは、塗料、インキ、あるいはプラス
チックスに配合されるが、このような塗布物あるいは成
型物の難燃化には寄与しない。近年このような塗布物あ
るいは成型物の難燃化が要求されてきた。この難燃化の
要求を満たす充填剤として、水酸化アルミニウム、酸化
アンチモンなどの粉末が用いられているが、これらの粒
子は大きく難燃性の効果は今−歩である。Particulate titanium dioxide is incorporated into paints, inks, or plastics, but it does not contribute to flame retardation of such coated products or molded products. In recent years, there has been a demand for flame retardant coatings or molded articles. Powders of aluminum hydroxide, antimony oxide, and the like are used as fillers to meet this flame retardant requirement, but these particles are large and their flame retardant effects are limited.
本発明のＨ的は、光に対して安定であり透明性及び紫外
線遮蔽性を損なうことなく、又、難燃性を有する酸化ア
ンチモンを被覆及び／又は粒子内部に含有した微粒子二
酸化チタン組成物及びその製造方法を提供することにあ
る。The object of the present invention is a fine particle titanium dioxide composition coated with and/or containing antimony oxide which is stable to light and has flame retardant properties without impairing transparency and ultraviolet shielding properties; The object of the present invention is to provide a manufacturing method thereof.
本発明によれば、最大粒径０．１μ以下、好ましくは０
．０３〜０．０７μの微粒子二酸化チタンを用い、該微
粒子二酸化チタンにアンチモン酸化物あるいは水酸化物
をＳｂ２Ｏ．として二酸化チタンの重量に対し、０．１
〜５０％含有させた微粒子二酸化チタンが提供される。According to the invention, the maximum particle size is 0.1μ or less, preferably 0.
．． Sb2O. 0.1 to the weight of titanium dioxide as
Particulate titanium dioxide containing ~50% is provided.
最大粒径が０．１μ以下であると、可視光線に対しては
透明性を有し、紫外線に対しては吸収及び散乱を生じる
ことはよく知られているが、粒子径が極めて小さい為に
当然の事ながら比表面積は著しく大きくなる。この比表
面積増大の為に、酸化チタンの光に対する活性度は顔料
紙の二酸化チタンに比較して極めて大きくなる。例えば
、エタノールの水溶液中に粒径が０．０５μのルチル型
の未処理の微粒子酸化チタン、同じくルチル型の顔料ク
ラスの未処理二酸化チタンをそれぞれ懸濁させ、３００
ｍμ〜８００ｍμの波長をもつ光線を水銀ランプによっ
て１６時間照射したところ、エタノールが分解した。こ
の分解率をガスクロマトグラフィーで測定したところ、
微粒子二酸化チタンの分解率が７５％に対して顔料クラ
スの二酸化チタンの分解率は３０％であった。It is well known that when the maximum particle size is 0.1μ or less, it is transparent to visible light and absorbs and scatters ultraviolet light, but because the particle size is extremely small, Naturally, the specific surface area becomes significantly larger. Due to this increase in specific surface area, the activity of titanium oxide against light becomes extremely large compared to the titanium dioxide of pigment paper. For example, rutile-type untreated fine particle titanium oxide with a particle size of 0.05μ and untreated titanium dioxide also in the rutile-type pigment class are suspended in an aqueous solution of ethanol.
When irradiated with light having a wavelength of mμ to 800 mμ for 16 hours using a mercury lamp, ethanol was decomposed. When this decomposition rate was measured by gas chromatography, it was found that
The decomposition rate of fine particle titanium dioxide was 75%, while the decomposition rate of pigment class titanium dioxide was 30%.
以上のように、微粒子二酸化チタンは光、特に紫外線に
対して活性度が高いことがわかった。これを改善すべく
、アンチモンを含有させることにより、著しく改善され
ることを見い出した。As described above, it was found that particulate titanium dioxide has high activity against light, especially ultraviolet light. In order to improve this, it has been found that by incorporating antimony, this can be significantly improved.
その製造方法は、例えば特開昭５９−２２３２３１によ
りつくられた微粒子酸化チタンを水中に攪拌しながら懸
濁させ、三塩化アンチモンの塩酸酸性水溶液を所望のア
ンチモン添加量となるように加える。その後、ｐＨ６〜
８になるように例えばアンモニア水、水酸化ナトリウム
水溶液などの塩基を加え調節する。その後公知の方法に
従って、口過、洗浄を行い、得られたケーキを乾燥する
。The manufacturing method is such that fine particles of titanium oxide prepared in, for example, JP-A-59-223231 are suspended in water with stirring, and an acidic aqueous solution of antimony trichloride in hydrochloric acid is added to the suspension to obtain the desired amount of antimony added. After that, pH 6~
8 by adding a base such as aqueous ammonia or aqueous sodium hydroxide solution. Thereafter, the cake is filtered and washed according to a known method, and the resulting cake is dried.
この状態では、アンチモン水和物が粒子表面に被覆され
たものが得られる。更にこれを所定の温度で焙焼しても
よい。この温度は通常８００℃以下の温度である。この
際、焙焼温度は、ベースとなる微粒子二酸化チタン粉末
の形成温度より低い温度であれば酸化チタン自身の粒子
の成長はなく、表面に酸化アンチモンあるいはその水和
物で被覆されたものが得られる。In this state, particles whose surfaces are coated with antimony hydrate are obtained. Furthermore, this may be roasted at a predetermined temperature. This temperature is usually below 800°C. At this time, if the roasting temperature is lower than the formation temperature of the base fine particle titanium dioxide powder, the particles of titanium oxide itself will not grow and a product whose surface is coated with antimony oxide or its hydrate will be obtained. It will be done.
焙焼温度がベースとなる微粒子二酸化チタン粉末の形成
温度より高い場合、微粒子二酸化チタンの粒子成長と共
に、アンチモン酸化物及び／又は水酸化物の形で微粒子
二酸化チタンの粒子表面を被覆すると同時に、微粒子二
酸化チタンの粒子内部にも含まれることとなる。When the roasting temperature is higher than the formation temperature of the base fine-particle titanium dioxide powder, as the fine-particle titanium dioxide grows, the surface of the fine-particle titanium dioxide is coated with antimony oxide and/or hydroxide, and at the same time, the fine-particles grow. It is also contained inside the particles of titanium dioxide.
また、ベースとなる微粒子二酸化チタンに周期律表■族
の化合物、Ｂ、ＡＩ、Ｇａ、Ｉｎの元素化合物が含まれ
ていると一層耐光性が向上する効果を有する。Further, if the base fine particle titanium dioxide contains a compound of group (I) of the periodic table, or a compound of elements such as B, AI, Ga, and In, the light resistance is further improved.
焙焼温度が８００℃を越えると二酸化チタン自身の成長
が増大しすぎて、もはや微粒子二酸化チタンでなくなり
、透明性及び紫外線遮蔽性は著しく減少する。When the roasting temperature exceeds 800°C, the growth of titanium dioxide itself increases so much that it is no longer particulate titanium dioxide, and the transparency and ultraviolet shielding properties are significantly reduced.
本発明による、アンチモン含有微粒子酸化チタンは光に
対して、著しく安定であり、且つ透明性及び紫外線遮蔽
性を有する。又、これをプラスチック板に練り込んだも
のの難燃化の試験の結果、同一条件下での従来の微粒子
二酸化チタン練り込み板に比較してより大きな効果があ
った。The antimony-containing fine particle titanium oxide according to the present invention is extremely stable to light, and has transparency and ultraviolet shielding properties. Further, as a result of a flame retardant test of a plastic plate kneaded with this material, it was found to have a greater effect than a conventional plate into which particulate titanium dioxide was kneaded under the same conditions.
実施例１
特開昭５９−２２３２３１の方法に従って得た平均粒子
径２３ｍμの微粒子二酸化チタン１０００ｇを水に懸濁
させて２０１とし、５０ｇ／ｌとなるよう調節した。こ
の懸濁液に、微粒子二酸化チタンに対して５ｂｚＯｉ
として１％となるように三塩化アンチモン塩酸酸性水溶
液（このものは４Ｎ塩酸水溶液１０００ ｍｌｌに５ｂ
Ｃ１，として１１７．１ ｇを溶解した水溶液）１３４
ＩＩ１１を１時間かけて滴下し、その後アンモニア水で
中和した。生成物を口過、洗浄後、乾燥し、６００℃で
２時間焙焼した。Example 1 1000 g of fine titanium dioxide having an average particle diameter of 23 mμ obtained according to the method of JP-A-59-223231 was suspended in water to give 201, and the concentration was adjusted to 50 g/l. This suspension contains 5bzOi for particulate titanium dioxide.
Antimony trichloride hydrochloric acid acidic aqueous solution (this is 5b in 1000 ml of 4N hydrochloric acid aqueous solution) to make 1%
Aqueous solution in which 117.1 g of C1 was dissolved) 134
II11 was added dropwise over 1 hour, and then neutralized with aqueous ammonia. The product was passed through the mouth, washed, dried, and roasted at 600°C for 2 hours.
得られた焙焼物をニックアトマイザ−で粉砕し、アンチ
モンを含有する平均粒子径０．０３５μの微粒子酸化チ
タンを得た。The obtained roasted product was pulverized with a nick atomizer to obtain fine particles of titanium oxide containing antimony and having an average particle diameter of 0.035 μm.
このものを塩化ビニル樹脂に練り込み硬質塩ビ板を作成
し、ウエザオメーターで３０時間照射し、取り出したテ
ストピースを色差計でり、ａ、ｂ値をそれぞれ照射前後
で測定し、これらの差を△Ｌ。This material was kneaded into vinyl chloride resin to create a hard PVC board, which was irradiated with a weatherometer for 30 hours.The test piece was taken out with a color difference meter and the a and b values were measured before and after irradiation, and the difference between them was determined. △L.
として求めた。I asked for it as.
この結果を比較例Ｉの結果と共に第１表に示した。The results are shown in Table 1 together with the results of Comparative Example I.
硬質塩ビ板は下記の条件で作成した。The hard PVC board was created under the following conditions.
配合
ゼオン１０３ＥＰ １００部安定剤
三塩基性硫酸鉛 １部二塩基性亜リン酸鉛
１部
二塩基性ステアリン酸鉛 １部
微粒子二酸化チタン １．０部加熱２本
ロールで混練後、厚み５間硬質塩ビ板を作成した。Compound Zeon 103EP 100 parts stabilizer
Tribasic lead sulfate 1 part Dibasic lead phosphite 1 part Dibasic lead stearate 1 part Particulate titanium dioxide 1.0 part After kneading with two heated rolls, a hard PVC board with a thickness of 5 mm was prepared.
また同様に塩化ビニル樹脂に練り込み、塩化ビニル樹脂
薄膜を作成した。この薄膜を、分光光度計（島原製作所
製、ＵＶ−２００）を使用して光の透過率を測定した。Similarly, it was kneaded into vinyl chloride resin to create a vinyl chloride resin thin film. The light transmittance of this thin film was measured using a spectrophotometer (manufactured by Shimabara Seisakusho, UV-200).
透明性、紫外線遮蔽性は比較例１のものに比較しても、
劣らぬものであった。Transparency and ultraviolet shielding properties are even compared to those of Comparative Example 1.
It was no less.
その結果を第１図に示す。The results are shown in FIG.
塩化ビニル樹脂薄膜は下記の条件で作成した。A vinyl chloride resin thin film was created under the following conditions.
配合
ゼオン１０３ＥＰ ６６部ステアリン酸バ
リウム １．９部ステアリン酸カドミウム
１．９部スズ系安定剤ＫＳ−２０１，９部
可塑剤ＤＯＰ ３０部
微粒子二酸化チタン ０．２５部加熱二本ロール
で混練後１００μの薄膜に成型する。Compound Zeon 103EP 66 parts Barium stearate 1.9 parts Cadmium stearate
1.9 parts Tin stabilizer KS-201, 9 parts Plasticizer DOP 30 parts Fine particle titanium dioxide 0.25 parts After kneading with two heated rolls, it is formed into a 100 μm thin film.
比較例１
実施例１の平均粒子径２３ｍμの微粒子酸化チタンに、
アンチモンを添加して乾燥するまでの工程を除いては、
実施例１と同様に処理して微粒子二酸化チタンを作成し
た。Comparative Example 1 The fine particle titanium oxide of Example 1 with an average particle diameter of 23 mμ,
Except for the process of adding antimony and drying,
Fine particles of titanium dioxide were prepared in the same manner as in Example 1.
（以下余白） 第 １ 表(Margin below) Chapter 1 Table
第１図は実施例１のアンチモン含有二酸化チタンを含有
するポリ塩化ビニルフィルムと、比較例工の製品を含有
するポリ塩化ビニルフィルムの光透過率のグラフである
。
特許出願人 帝国化工株式会社FIG. 1 is a graph of the light transmittance of the polyvinyl chloride film containing antimony-containing titanium dioxide of Example 1 and the polyvinyl chloride film containing the product of Comparative Example. Patent applicant Teikoku Kako Co., Ltd.
Claims (2)
及び／又は粒子内部にアンチモンの酸化物及び／又は水
酸化物をＳｂ＿２Ｏ＿３として二酸化チタンの重量を基
準として０．１〜５０％被覆及び／又は含有させてなる
微粒子二酸化チタン粉末。(1) The maximum particle size is 0.1μ or less, and the particle surface and/or inside the particle is coated with antimony oxide and/or hydroxide in an amount of 0.1 to 50% as Sb_2O_3 based on the weight of titanium dioxide. and/or fine particle titanium dioxide powder.
水懸濁液へ、二酸化チタンの重量を基準としてＳｂ＿２
Ｏ＿３として０．１〜５０％の水溶性アンチモン化合物
を添加し、次いで該懸濁液をｐＨ６〜８になるように中
和することにより水酸化アンチモンの被覆層を形成し、
被覆した懸濁粒子をロ過、水洗及び乾燥し、次いで８０
０℃以下の温度で焼成することを特徴とするアンチモン
含有微粒子二酸化チタン粉末の製造法。(2) Sb_2 based on the weight of titanium dioxide to a fine particle titanium dioxide aqueous suspension with a maximum particle size of 0.1μ or less
A coating layer of antimony hydroxide is formed by adding 0.1 to 50% of a water-soluble antimony compound as O_3, and then neutralizing the suspension to a pH of 6 to 8.
The coated suspended particles were filtered, washed and dried, then
A method for producing antimony-containing fine-particle titanium dioxide powder, which comprises firing at a temperature of 0°C or lower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1333989A JPH02194064A (en) | 1989-01-20 | 1989-01-20 | Antimony-containing fine particle titanium dioxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1333989A JPH02194064A (en) | 1989-01-20 | 1989-01-20 | Antimony-containing fine particle titanium dioxide powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02194064A true JPH02194064A (en) | 1990-07-31 |
Family
ID=11830369
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1333989A Pending JPH02194064A (en) | 1989-01-20 | 1989-01-20 | Antimony-containing fine particle titanium dioxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02194064A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0579062A3 (en) * | 1992-07-11 | 1994-08-03 | Kronos Titan Gmbh | |
| JP2006298731A (en) * | 2005-04-25 | 2006-11-02 | Mitsui Chemicals Inc | Compound oxide ultrafine particle and method for manufacturing the same |
| JP2014065988A (en) * | 2012-09-26 | 2014-04-17 | Oji Holdings Corp | Decorative board base-paper |
| CN111363386A (en) * | 2020-05-11 | 2020-07-03 | 华东理工大学 | A kind of preparation method of titanium dioxide for nylon chemical fiber extinction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5580467A (en) * | 1978-11-30 | 1980-06-17 | Du Pont | Light stable titanium dioxide pigment composition |
| JPS57167357A (en) * | 1981-04-08 | 1982-10-15 | Ishihara Sangyo Kaisha Ltd | Production of titanium dioxide pigment |
| JPH01264932A (en) * | 1988-04-15 | 1989-10-23 | Ishihara Sangyo Kaisha Ltd | Acicular titanium dioxide having characteristic required for pigment and its production |
-
1989
- 1989-01-20 JP JP1333989A patent/JPH02194064A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5580467A (en) * | 1978-11-30 | 1980-06-17 | Du Pont | Light stable titanium dioxide pigment composition |
| JPS57167357A (en) * | 1981-04-08 | 1982-10-15 | Ishihara Sangyo Kaisha Ltd | Production of titanium dioxide pigment |
| JPH01264932A (en) * | 1988-04-15 | 1989-10-23 | Ishihara Sangyo Kaisha Ltd | Acicular titanium dioxide having characteristic required for pigment and its production |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0579062A3 (en) * | 1992-07-11 | 1994-08-03 | Kronos Titan Gmbh | |
| JP2006298731A (en) * | 2005-04-25 | 2006-11-02 | Mitsui Chemicals Inc | Compound oxide ultrafine particle and method for manufacturing the same |
| JP2014065988A (en) * | 2012-09-26 | 2014-04-17 | Oji Holdings Corp | Decorative board base-paper |
| CN111363386A (en) * | 2020-05-11 | 2020-07-03 | 华东理工大学 | A kind of preparation method of titanium dioxide for nylon chemical fiber extinction |
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