JPH04154622A - Production of white bismuth oxide composition - Google Patents
Production of white bismuth oxide compositionInfo
- Publication number
- JPH04154622A JPH04154622A JP2275450A JP27545090A JPH04154622A JP H04154622 A JPH04154622 A JP H04154622A JP 2275450 A JP2275450 A JP 2275450A JP 27545090 A JP27545090 A JP 27545090A JP H04154622 A JPH04154622 A JP H04154622A
- Authority
- JP
- Japan
- Prior art keywords
- bismuth oxide
- bismuth
- slurry
- oxide composition
- white
- 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.)
- Granted
Links
- 229910000416 bismuth oxide Inorganic materials 0.000 title claims abstract description 24
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 239000000203 mixture Substances 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title claims 2
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 6
- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical class S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000003518 caustics Substances 0.000 claims abstract description 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000002872 contrast media Substances 0.000 abstract description 9
- 239000002245 particle Substances 0.000 abstract description 8
- 238000000354 decomposition reaction Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract description 3
- 238000000926 separation method Methods 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 abstract 1
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 12
- 239000003153 chemical reaction reagent Substances 0.000 description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 8
- 239000000047 product Substances 0.000 description 7
- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 description 4
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 4
- 150000001622 bismuth compounds Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 2
- -1 % by weight Chemical compound 0.000 description 1
- 229910000014 Bismuth subcarbonate Inorganic materials 0.000 description 1
- HWSISDHAHRVNMT-UHFFFAOYSA-N Bismuth subnitrate Chemical compound O[NH+]([O-])O[Bi](O[N+]([O-])=O)O[N+]([O-])=O HWSISDHAHRVNMT-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 1
- MGLUJXPJRXTKJM-UHFFFAOYSA-L bismuth subcarbonate Chemical compound O=[Bi]OC(=O)O[Bi]=O MGLUJXPJRXTKJM-UHFFFAOYSA-L 0.000 description 1
- 229940036358 bismuth subcarbonate Drugs 0.000 description 1
- 229960001482 bismuth subnitrate Drugs 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 230000000747 cardiac effect Effects 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000002594 fluoroscopy Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 230000002792 vascular Effects 0.000 description 1
Landscapes
- Medicines Containing Antibodies Or Antigens For Use As Internal Diagnostic Agents (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
血管カテーテル等の医療器具に造影剤として使用される
酸化ビスマスに関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to bismuth oxide used as a contrast agent in medical instruments such as vascular catheters.
［従来の技術］
近時、Ｘ線透視下で用いられる心臓カテーテル等の医療
器具の発達は目覚しく、各種の器具が開発されている。[Prior Art] In recent years, medical instruments such as cardiac catheters used under X-ray fluoroscopy have made remarkable progress, and various instruments have been developed.
これらの器具は、テフロン、ポリウレタン等に造影剤と
しての硫酸バリウムとを混練し、成形し、作成していた
が、造影剤として硫酸バＩＪ ラムを使用する際には、
所定の造影効果を得るためには樹脂量に対し４０〜６０
重量％といった多量の硫酸バリウムを樹脂に加える必要
がある。しかし、そうすると樹脂の特性が極めて悪化し
て医療器具として使用に堪えないものとなってしまう。These instruments were made by kneading Teflon, polyurethane, etc. with barium sulfate as a contrast agent and molding them. However, when using barium sulfate as a contrast agent,
In order to obtain the desired contrast effect, the amount of resin should be 40 to 60%.
It is necessary to add a large amount of barium sulfate, such as % by weight, to the resin. However, in this case, the properties of the resin deteriorate significantly, making it unusable as a medical device.
このため、実際には造影効果を犠牲にし、樹脂が使用し
うるちのとなる範囲内で硫酸バリウムを添加していた。For this reason, in practice, barium sulfate was added to the resin within the range that could be used, at the expense of the contrast effect.
［発明が解決しようとする課題］
上記欠点を解消すべく、酸化ビスマスを主とするビスマ
ス化合物を硫酸バリウムの代用とする方法が提案され、
採用されている。これは、ビスマス化合物の造影効果が
硫酸バリウムの２倍強となるからである。しかし、従来
の酸化ビスマスは黄色であり、医療器具として好まれる
青色等に着色使用とすると色が濁るという問題がある。[Problems to be Solved by the Invention] In order to eliminate the above drawbacks, a method has been proposed in which a bismuth compound mainly consisting of bismuth oxide is used as a substitute for barium sulfate.
It has been adopted. This is because the contrast effect of bismuth compounds is more than twice that of barium sulfate. However, conventional bismuth oxide is yellow, and when it is used in a color such as blue, which is preferred for medical instruments, there is a problem that the color becomes cloudy.
これを避けるために白色ビスマス化合物であるオキシ塩
化ビスマス、次炭酸ビスマス、次硝酸ビスマス等を使用
しようとすると、これらのビスマス化合物は樹脂との混
線時の加熱により分解し、着色したり、ガスが発生した
りするばかりでなく、得られた製品を使用しようとする
と、人体に有害な酸等の溶出の可能性が高い等の問題が
ある。If you try to use white bismuth compounds such as bismuth oxychloride, bismuth subcarbonate, bismuth subnitrate, etc. to avoid this, these bismuth compounds will decompose due to heating when mixed with the resin, causing color and gas release. Not only that, but when trying to use the obtained product, there is a high possibility that acids and the like that are harmful to the human body will elute.
本発明は上記問題点のない造影剤用微粒白色酸化ビスマ
ス組成物の提供を目的とする。The object of the present invention is to provide a fine-grained white bismuth oxide composition for contrast agents that does not have the above-mentioned problems.
［課題を解決するための手段］
本発明者は白色酸化ビスマスの製造方法を種々検討した
結果、酸化ビスマスに硫酸根を一定量含有させることに
より造影剤として使用可能な白色酸化ビスマス組成物を
得ることを見出し本発明に至った。[Means for Solving the Problem] As a result of studying various methods for producing white bismuth oxide, the present inventor obtained a white bismuth oxide composition that can be used as a contrast agent by incorporating a certain amount of sulfate radical into bismuth oxide. This discovery led to the present invention.
すなわち、上記課題を解決する本発明の方法は、硝酸ビ
スマス溶液に苛性アルカリ溶液を加えてｐＨ６〜９とし
てスラリーを得、該スラリーに、スラリー中のビスマス
１モルに対して０．１６〜０．６０モルの過硫酸塩を添
加し、液温を６０〜９０℃、好ましくは７０〜９０℃に
維持しつつ、少なくとも１時間攪拌し、生成した殿物を
固液分離し、要すれば乾燥し、次いで４００〜６００℃
、好ましくは４５０〜５５０℃で焙焼するものである。That is, the method of the present invention for solving the above problems involves adding a caustic alkaline solution to a bismuth nitrate solution to adjust the pH to 6 to 9 to obtain a slurry, and adding 0.16 to 0.0. Add 60 mol of persulfate, stir for at least 1 hour while maintaining the liquid temperature at 60-90°C, preferably 70-90°C, separate the formed precipitate into solid and liquid, and dry if necessary. , then 400-600℃
, preferably roasted at 450 to 550°C.
本発明に使用しうる苛性アルカリは水酸化ナトリウム、
水酸化カリウム、アンモニア、アンモニア水であり、そ
れぞれ単独あるいは混合して用いることができる。又、
使用しうる過硫酸塩は過硫酸ナトリウム、過硫酸カリ、
過硫酸アンモニウムであり、これもそれぞれ単独、ある
いは混合して使用しうる。The caustic alkali that can be used in the present invention is sodium hydroxide,
Potassium hydroxide, ammonia, and aqueous ammonia can be used alone or in combination. or,
Persulfates that can be used include sodium persulfate, potassium persulfate,
Ammonium persulfate can be used alone or in combination.
このようにして得られた白色酸化ビスマス組成物は、
式 （ＢｉＯｘ） ｚ ・（３−２Ｘ）ＳＯ４Ｘが１．
０８ ≦Ｘ ≦１．３６
で示され、平均粒径が０．５〜１０μｍ１白色度が９３
以上、黄色度が１１以下、分解温度がＳＯＯ℃以上で実
質的に無害であり、医療用器具のための造影剤として最
適である。なお、白色度はＪＩＳＺ ８７２０．８７２
２．８７２９に従い測定するものであり、黄色度はＪＩ
Ｓ Ｋ ７１０３に従い測定するものである。The white bismuth oxide composition thus obtained has the formula (BiOx) z .(3-2X)SO4X is 1.
08 ≦X ≦1.36, average particle size is 0.5 to 10 μm, whiteness is 93
As described above, it has a yellowness value of 11 or less and a decomposition temperature of SOO°C or more, making it substantially harmless and suitable as a contrast agent for medical instruments. In addition, the whiteness is JISZ 8720.872
2.8729, and the yellowness is determined according to JI
It is measured according to SK 7103.
［作用］
本発明において、酸化ビスマスを硝酸に溶解して得た硝
酸ビスマス溶液のｐＨを６〜９とするのは、ｐＨ６以下
では生成する反応生成物の粒径が１０μｍを越え、造影
剤として使用する際に樹脂と均一に混合できなくなるか
らであり、ｐＨが９を越えると後工程の焙焼で黄色に着
色するからである。[Function] In the present invention, the pH of the bismuth nitrate solution obtained by dissolving bismuth oxide in nitric acid is set to 6 to 9. If the pH is below 6, the particle size of the reaction product generated exceeds 10 μm, and it cannot be used as a contrast agent. This is because it cannot be uniformly mixed with the resin during use, and if the pH exceeds 9, it will be colored yellow during roasting in the subsequent process.
過硫酸アルカリの添加量をスラリー中のビスマス１モル
に対して０．１６〜０．６０モルとするのは、０．１６
モル以下では白色度が９３未満となり、黄色度が１１を
越えるからであり、０．６０モルを越えると反応に直接
関与しない過硫酸塩の量が増加し経済性を損うからであ
る。反応温度を６０〜９０℃とするのは、６０℃未満で
は十分な反応が起きず、９０°Ｃ以上に加熱しても反応
速度はそれ以上大きく増加せず、かえって取扱い上の危
険性が増し、経済性を損うからである。反応時間として
は少なくとも１時間が必要でありこれを下回る時には十
分な白色度の物が得られない。The amount of alkali persulfate added is 0.16 to 0.60 mol per 1 mol of bismuth in the slurry.
This is because if the amount is less than 0.60 mol, the whiteness will be less than 93 and the yellowness will be more than 11. If it exceeds 0.60 mol, the amount of persulfate that does not directly participate in the reaction will increase, impairing economic efficiency. The reason why the reaction temperature is set at 60 to 90°C is that sufficient reaction does not occur below 60°C, and even if heated above 90°C, the reaction rate does not increase any further, and on the contrary, the danger in handling increases. This is because it impairs economic efficiency. The reaction time is required to be at least 1 hour, and if the reaction time is shorter than this, a product with sufficient whiteness cannot be obtained.
この用にして得た殿物を焙焼するのは揮発物や分解しや
すい物を除去するためであり、このようにすることによ
り樹脂との混合時の分解生成物の発生を抑えるためであ
る。このため焙焼温度は４００℃以上としなければなら
ない。しかし、６００°Ｃを越えると白色酸化ビスマス
組成物が分解する。The precipitate obtained for this purpose is roasted in order to remove volatile substances and substances that are easily decomposed, and by doing so, it is possible to suppress the generation of decomposition products when mixed with resin. . For this reason, the roasting temperature must be 400°C or higher. However, when the temperature exceeds 600°C, the white bismuth oxide composition decomposes.
このため焙焼温度は４００〜６００℃とすることが必要
である。For this reason, it is necessary to set the roasting temperature to 400 to 600°C.
［実施例−１］
試薬１級の酸化ビスマス（和光純薬製）７５ｇを６２％
硝酸１４４ ｍｌに溶解し、次いで、該溶液に純水５０
０１ と試薬１級の濃アンモニア水でｐＨ６，２２に中
和した。生成したスラリー中に試薬１級の過硫酸アンモ
ニウム３０．５ｇを添加し、８０°Ｃで２時間攪拌し、
ろ別して乾燥し、黄色の沈殿を得、これを乾燥して大気
中５００℃で２時間ぽい焼して８０ｇの白色の酸化ビス
マス組成物を得た。組成分析の結果この生成物はｘ ＝
１．１０の（ＢｉＯｘ） ｚ ・（３−２Ｘ）ＳＯ２
であった。[Example-1] 62% of 75 g of first class reagent bismuth oxide (manufactured by Wako Pure Chemical Industries)
Dissolve in 144 ml of nitric acid, then add 50 ml of pure water to the solution.
01 and reagent grade 1 concentrated ammonia water to pH 6.22. 30.5 g of ammonium persulfate of the first class reagent was added to the generated slurry, and the mixture was stirred at 80°C for 2 hours.
It was filtered and dried to obtain a yellow precipitate, which was dried and calcined in the air at 500° C. for 2 hours to obtain 80 g of a white bismuth oxide composition. As a result of compositional analysis, this product is x =
1.10 (BiOx)z ・(3-2X)SO2
Met.
この組成物の白色度と黄色度とを東京電色製デジタルカ
ラーメーターＴＣ−３６０Ｕで求めたところ、それぞれ
９７．７．５であり、走査電子顕微鏡写真より求めた平
均粒径は５μｍであった。The whiteness and yellowness of this composition were determined using a Tokyo Denshoku digital color meter TC-360U, and were each 97.7.5, and the average particle size determined from a scanning electron micrograph was 5 μm. .
［実施例−２１
試薬１級の酸化ビスマス（和光純薬製）７５ｇを６２％
硝酸１４４ ｍｌに溶解し、次いで、該溶液に純水５０
０ ｍｌを添加し、試薬１級の水酸化ナトリウムでｐＨ
を７．１１にした。生成したスラリー中に試薬１級の過
硫酸ナトリウム３０．６ｇを添加し、８０°Ｃで２時間
攪拌し、ろ別して乾燥し、黄土色の沈殿を得、これを乾
燥して大気中５００００で２時間ぽい焼して７８ ｇの
白色の酸化ビスマス組成物を得た。組成分析の結果この
生成物はＸ＝１．２４の（ＢｔＯｘ） ｓ ・（３−２
Ｘ）ＳＯ４であった。[Example-21 75g of reagent grade 1 bismuth oxide (manufactured by Wako Pure Chemical Industries, Ltd.) at 62%
Dissolve in 144 ml of nitric acid, then add 50 ml of pure water to the solution.
Add 0 ml and adjust the pH with reagent grade 1 sodium hydroxide.
was set to 7.11. 30.6 g of reagent grade 1 sodium persulfate was added to the resulting slurry, stirred at 80°C for 2 hours, filtered and dried to obtain an ocher colored precipitate. After baking for an hour, 78 g of a white bismuth oxide composition was obtained. As a result of compositional analysis, this product is (BtOx) s ・(3-2
X) It was SO4.
この組成物の白色度と黄色度とを東京重色製デジタルカ
ラーメーターＴＣ−３６０Ｕで求めたところ、それぞれ
９６．８．７であり、走査電子顕微鏡写真より求めた平
均粒径は５μｍであった。When the whiteness and yellowness of this composition were determined using a digital color meter TC-360U manufactured by Tokyo Juishiki Co., Ltd., they were each 96.8.7, and the average particle size determined from a scanning electron micrograph was 5 μm. .
［実施例−３コ
試薬１級の酸化ビスマス（和光純薬製）７５ｇを６２
％硝酸１４４１に溶解し、次いで、該溶液に純水５００
ｍｌを添加し、試薬１級の濃アンモニア水でｐＨを８
．２５にした。生成したスラリー中に試薬１級の過硫酸
アンモニウム３６．４ｇを添加し、７０℃で２時間攪拌
し、ろ別して乾燥し、茶色の沈殿を得、これを乾燥して
大気中４５０℃で２時間ぽい焼して７６ ｇの白色の酸
化ビスマス組成物を得た。組成分析の結果この生成物は
ｘ＝１．３０の （ＢｉＯｘ）＊ ・（３−２ｘ）ＳＯ
４であった。[Example-3] 75 g of reagent grade 1 bismuth oxide (manufactured by Wako Pure Chemical Industries, Ltd.) was
Dissolved in 1441% nitric acid, then added 500% pure water to the solution.
ml and adjust the pH to 8 with reagent grade 1 concentrated ammonia water.
．． I made it 25. 36.4 g of ammonium persulfate of the first class reagent was added to the resulting slurry, stirred at 70°C for 2 hours, filtered and dried to obtain a brown precipitate, which was dried in the atmosphere at 450°C for 2 hours. Calcination yielded 76 g of a white bismuth oxide composition. As a result of compositional analysis, this product is (BiOx)* ・(3-2x)SO with x=1.30
It was 4.
この組成物の白色度と黄色度とを東京重色製デジタルカ
ラーメーターＴＣ−３６０Ｕで求めたところ、それぞれ
９４．１０．０であり、走査電子顕微鏡写真より求めた
平均粒径は０．５μ■であった。The whiteness and yellowness of this composition were determined using a digital color meter TC-360U manufactured by Tokyo Juishiki Co., Ltd., and were 94.10.0, respectively, and the average particle size determined from a scanning electron micrograph was 0.5μ■ Met.
［比較例コ
試薬１級の酸化ビスマス（和光純薬製）７５ｇを６２％
硝酸１４４■ｌに溶解し、次いで、該溶液に純水５００
ｍｌを添加し、試薬１級の濃アンモニア水でｐＨを９
．５４にした。生成したスラリー中に試薬１級の過硫酸
アンモニウム３０．５ｇを添加し、８０℃で２時間攪拌
し、ろ別して乾燥し、レンガ色の沈殿を得、これを乾燥
して大気中４５０℃で２時間ぽい焼して７４ ｇの白色
の酸化ビスマス組成物を得た。組成分析の結果この生成
物はｘ＝１．４３の（ＢｉＯｌ［）ａ・（３−２ｘ）Ｓ
Ｏ，であった。[Comparative Example: 75g of reagent grade 1 bismuth oxide (manufactured by Wako Pure Chemical Industries, Ltd.) was added to 62%
Dissolve in 144 μl of nitric acid, then add 500 μl of pure water to the solution.
ml and adjust the pH to 9 with reagent grade 1 concentrated ammonia water.
．． I made it 54. 30.5 g of ammonium persulfate of grade 1 reagent was added to the resulting slurry, stirred at 80°C for 2 hours, filtered and dried to obtain a brick-colored precipitate, which was dried in the atmosphere at 450°C for 2 hours. After roasting, 74 g of white bismuth oxide composition was obtained. As a result of compositional analysis, this product is (BiOl[)a・(3-2x)S with x=1.43
It was O.
この組成物の白色度と黄色度とを東京重色製デジタルカ
ラーメーターＴＣ−３６０Ｕで求めたところ、それぞれ
８８．１５．０であり、走査電子顕微鏡写真より求めた
平均粒径は４μ嘗であった。The whiteness and yellowness of this composition were determined using a digital color meter TC-360U manufactured by Tokyo Juishiki Co., Ltd., and were 88.15.0, respectively, and the average particle size determined from a scanning electron micrograph was 4 μm. Ta.
［発明の効果］
本発明の方法に従えば、容易に
式（ＢｉＱｘ）、・（３−２ｘ）ＳＯ４Ｘが１．０８≦
Ｘ≦１，３６
で示され、平均粒径が０．５〜ｌＯμｍ、白色度が９３
以上、黄色度が１１以下、分解温度が５００°Ｃ以上で
実質的に無害であり、医療用器具のための造影剤として
最適である白色酸化ビスマス組成物を得ることができる
。[Effects of the Invention] According to the method of the present invention, the formula (BiQx), ・(3-2x)SO4X can be easily set to 1.08≦
X≦1,36, the average particle size is 0.5 to 10 μm, and the whiteness is 93
As described above, it is possible to obtain a white bismuth oxide composition that has a yellowness of 11 or less, a decomposition temperature of 500° C. or more, is substantially harmless, and is optimal as a contrast agent for medical instruments.
特許出願人 住友金属鉱山株式会社Patent applicant: Sumitomo Metal Mining Co., Ltd.
Claims (1)
〜９としてスラリーを得、該スラリーに、スラリー中の
ビスマス１モルに対して０．１６〜０．６０モルの過硫
酸塩を添加し、液温を６０〜９０℃に維持しつつ、少な
くとも１時間攪拌し、生成した殿物を固液分離し、次い
で４００〜６００℃で焙焼することを特徴とする白色酸
化ビスマス組成物の製造方法。Add caustic alkaline solution to bismuth nitrate solution to pH 6
A slurry is obtained as 9 to 9, and 0.16 to 0.60 mol of persulfate is added to the slurry per 1 mol of bismuth in the slurry, and while maintaining the liquid temperature at 60 to 90°C, at least 1 A method for producing a white bismuth oxide composition, which comprises stirring for a period of time, separating the produced precipitate into solid and liquid, and then roasting at 400 to 600°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2275450A JPH0761872B2 (en) | 1990-10-16 | 1990-10-16 | Method for producing white bismuth oxide composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2275450A JPH0761872B2 (en) | 1990-10-16 | 1990-10-16 | Method for producing white bismuth oxide composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04154622A true JPH04154622A (en) | 1992-05-27 |
| JPH0761872B2 JPH0761872B2 (en) | 1995-07-05 |
Family
ID=17555700
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2275450A Expired - Lifetime JPH0761872B2 (en) | 1990-10-16 | 1990-10-16 | Method for producing white bismuth oxide composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0761872B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995006053A1 (en) * | 1993-08-23 | 1995-03-02 | Nissan Chemical Industries, Ltd. | Tris(substituted phenyl)bismuth derivative |
| JPH111322A (en) * | 1997-06-10 | 1999-01-06 | Dowa Mining Co Ltd | Bismuth oxide powder and its production |
-
1990
- 1990-10-16 JP JP2275450A patent/JPH0761872B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1995006053A1 (en) * | 1993-08-23 | 1995-03-02 | Nissan Chemical Industries, Ltd. | Tris(substituted phenyl)bismuth derivative |
| JPH111322A (en) * | 1997-06-10 | 1999-01-06 | Dowa Mining Co Ltd | Bismuth oxide powder and its production |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0761872B2 (en) | 1995-07-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0828690B1 (en) | Spheroidally agglomerated basic cobalt (ii) carbonate and spheroidally agglomerated cobalt (ii) hydroxide, process for their production and their use | |
| JP2815611B2 (en) | Method for producing manganese oxide | |
| JPH0323220A (en) | Preparation of white electrically- conductive zinc oxide | |
| JPH04154622A (en) | Production of white bismuth oxide composition | |
| JPH06279347A (en) | Alkali earth potassium acetate, preparation and use thereof | |
| JPS62207716A (en) | Manufacture of copper hydroxide | |
| JP4236015B2 (en) | Novel Ca / Mg composite carbonates, process for producing the same, and antacid | |
| JP2506479B2 (en) | White bismuth oxide composition | |
| JPS6183627A (en) | Production of powdery zirconium oxide | |
| JPS59223204A (en) | Spherical anhydrous calcium secondary phosphate | |
| JPH05270831A (en) | White bismuth oxide and its production | |
| JPH02208227A (en) | Production of low-bulk density tricobalt tetroxide | |
| JPH03200878A (en) | Preparation of powder coated with zinc oxide | |
| JP2592563B2 (en) | Method for producing octacalcium phosphate | |
| US3004832A (en) | Process for producing titanium carbide | |
| JPS5867644A (en) | Stabilizing method of basic aluminum lactate | |
| JPS61132519A (en) | Production of bismuth oxide fine powder | |
| JP3505133B2 (en) | Surface conductive nickel oxyhydroxide and method for producing the same | |
| JPH01278417A (en) | Novel reactive derivative of zirconium and method for its manufacture | |
| JP2736693B2 (en) | Method for producing jarosite particle powder | |
| JP2524893B2 (en) | Antibacterial / antifungal phosphate double salt and method for producing the same | |
| JP3022607B2 (en) | Production of free-flowing hydrated ferrous sulfate. | |
| US3442607A (en) | Antimony tetroxide production | |
| JPH02311318A (en) | Production of tricobalt tetroxide | |
| JPS62241805A (en) | Production of chlorine |