TW524774B - Bactericidal silicon dioxide doped with silver - Google Patents

Bactericidal silicon dioxide doped with silver Download PDF

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TW524774B
TW524774B TW089118153A TW89118153A TW524774B TW 524774 B TW524774 B TW 524774B TW 089118153 A TW089118153 A TW 089118153A TW 89118153 A TW89118153 A TW 89118153A TW 524774 B TW524774 B TW 524774B
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Taiwan
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silver
doped
silicon dioxide
aerosol
oxide
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TW089118153A
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Helmut Mangold
Rainer Golchert
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Degussa
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
    • A01N59/16—Heavy metals; Compounds thereof
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K6/00—Preparations for dentistry
    • A61K6/70—Preparations for dentistry comprising inorganic additives
    • A61K6/71—Fillers
    • A61K6/76—Fillers comprising silicon-containing compounds
    • A—HUMAN NECESSITIES
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    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/25—Silicon; Compounds thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
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    • A61L2/16—Methods or apparatus for disinfecting or sterilising materials or objects other than foodstuffs or contact lenses; Accessories therefor using chemical substances
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    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q11/00—Preparations for care of the teeth, of the oral cavity or of dentures; Dentifrices, e.g. toothpastes; Mouth rinses
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
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    • B01J35/31—Density
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    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/615—100-500 m2/g
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027—Powdering
    • B01J37/0054—Drying of aerosols
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
    • C01B33/181—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process
    • C01B33/183—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by a dry process by oxidation or hydrolysis in the vapour phase of silicon compounds such as halides, trichlorosilane, monosilane
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Description

524774 A7 B7 經濟部智慧財產局員工消費合作社印製 1、發明説明（1 ) 本發明係關於藉氣溶膠摻雜銀或氧化銀之於高熱下製 得的二氧化矽，其具有殺菌性質，及關於其製法和用途。 亦係關於其於分散液中或在橡膠和矽酮橡膠中作爲塡料之 使用。 已經知道在火燄中使用特殊方法以一個步驟摻雜於高 熱製得的二氧化矽（DE 96 50 500 A 1)。此方法合倂高溫火 燄水解及熱解反應。此摻雜法與所謂的”共熔融法，，不同，其 中，氣態起始材料（如：SiCl4氣體和AlCh氣體）先混合，並 於火燄反應器中一起燃燒。 摻雜法中，氣溶膠引至火燄中，其中，火成氧化物藉 火燄水解法製得，此氣溶膠含有欲摻雜化合物的鹽.類。 現已經知道：如果使用溶解於水中的銀鹽作爲氣溶膠 的起始物，所得產物是具有殺菌性之經摻雜的火成二氧化 本發明提出一種藉氣溶膠摻入銀或氧化銀之於高溫製 得的二氧化矽，其中，此二氧化矽的特點在於：基礎組份 是以火燄氧化或火燄水解方式（以後者爲佳）於高熱下製得的 二氧化矽，此二氧化矽摻有lxl0·4至20重量％的摻雜組份， 摻雜量以在1至1 0,000PPm範圍內爲佳，摻雜組份是銀化合 物或金屬銀的鹽或鹽混合物或它們的混合物，經摻雜的氧 化物之BET表面積由1至600平方米/克，以在40至400平方 米/克範圍內爲佳。 本發明另提出一種製備藉氣溶膠摻雜銀或氧化銀之於 高熱下製得之二氧化矽的方法，此方法的特徵在於··氣溶 (請先閲讀背面之注意事項
本頁w 訂
本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -4 - 524774 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明（2 ) 膠進入用以藉火燄氧化或火燄水解方式（以後者爲佳）而於高 熱製備二氧化矽的火燄中，在反應之前，此氣溶膠與火燄 氧化反應或火燄水解反應的氣體混合物均勻混合，之後， 使氣溶膠/氣體混合物在火燄中反應，以已知方式，自氣 流中分離所得之摻有銀或氧化銀之於高熱製得的二氧化矽 ’以含有銀的鹽類或鹽混合物的鹽溶液或處於溶解或懸浮 形式的銀金屬或它們的混合物作爲氣溶膠起始物，此氣溶 膠可藉二組份噴嘴以霧化方式或藉其他產製氣溶膠的方法（ 以利用超音波霧化的氣溶膠產生器者爲佳）製得。 使用下列鹽類：AgN〇3、Ag2(S〇4)、Ag2〇及與錯合劑或 氨錯合者。 由 Ullmanns Enzyklopadie der techn. Chemie 4th edition，Vol.21，p.464知道用以製備火成氧化物的火談水 解法。 根據本發明之藉氣溶膠而摻有銀或氧化銀之於高熱製 得的火成二氧化矽可以作爲殺菌塡料，特別是用以產製塗 漆或塗料，用於紙業，作爲催化活性物質，作爲用以製造 分散物的起始物，作爲硏磨材料（CMP應用），作爲陶瓷原料 ’用於電子工業，作爲聚合物的塡料，作爲製造玻璃或玻 璃塗料或玻璃纖維的起始物，作爲亦可於高溫使用的脫模 助劑，用於化粧品工業，作爲吸收劑材料，作爲矽酮和橡 膠工業的添加物，用以調整液體系統的流變性，用於熱保 護安定作用’作爲隔熱材料，作爲流動助劑，作爲牙科用 塡料，在醫藥工業中作爲輔助劑，用於塗料工業。 (請先閲讀背面之注意事項vW寫本頁)， 1 裝- 訂 .¾ ΙΓ, 本紙張尺度適用中國國家標準（CNS )八4規格（noX 297公釐） -5 - 524774 經濟部智慧財產局員工消費合作社印製 A7 _ B7___五、發明説明（3 ) 本發明亦提出一種殺菌塡料，特別是用於塗漆和塗料 和紙業，其特徵在於其含括根據本發明之藉氣溶膠摻雜銀 或氧化的火成二氧化矽。 參考附圖1和下列實例，進一步描述根據本發明之經摻 雜的二氧化矽及其製法和用途。 附圖1所示者是摻雜裝置。此裝置的核心組件是用以製 備於火成氧化物之已知類型的燃燒器。附圖1中的1爲燃燒 器。 燃燒器1有中央管2，其開口進入噴嘴3，主要氣流由噴 嘴3流入燃燒室，於此處燃燒。內部噴嘴被另一環噴嘴4所 環繞，（環或次要）氫由噴嘴4流出。 中央管2中，有另一軸管5，其末端距離中央管2噴嘴數 公分。氣溶膠被引至軸管5中。 在氣溶膠產生器6(超音波霧化器）中製得由銀鹽的水溶 液構成的氣溶膠。 在氣溶膠產生器中製得的銀鹽/水氣溶膠藉由輕載氣 流通過加熱區7，伴隨的水於此區蒸發，留下氣相細粒形式 的小鹽晶體。 實例1 :摻有銀或氧化銀的火成二氧化矽之製備 4.44公斤/小時31(：14於約130艽蒸發並運送至已知類型 燃燒器的中央管。3立方米/小時的（主要）氫和7.5立方米/ 小時的空氣引至中央管中。 氣體混合物自燃燒器的內部噴嘴流出，在有水冷管位 (請先閱讀背面之注意事項寫本頁弋 _裝.
、1T
本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -6 - 524774 A7 B7 經濟部智慧財產局員工消費合作社印製 五、發明説明（4 ) 於附近的燃燒室中燃燒 0·5立方米/小時的（護套或次要）氫進入護套噴嘴。 另將12立方米/小時的空氣引至燃燒室中。 第二種氣體組份自軸管5流出，進入中央管2。 第二種氣流含括在獨立霧化單元中藉超音波霧化作用 製得的氣溶膠。氣溶膠產生器霧化7 2 5克/小時5 %硫酸銀水 溶液。此硫酸銀氣溶膠藉載氣（0.5立方米/小時空氣）之助 而被導引通過已受熱的管，含水的氣溶膠於約180 °C被轉化 成氣體和鹽晶體氣溶膠。 反應氣體和摻有銀或銀氧化物之所得的火成二氧化矽 因施用的低壓而被導引通過冷卻系統，顆粒氣流藉此冷卻 至約100至160°C。在濾器或旋風機中自廢氣流分離此固體 〇 得到之摻有銀（氧化物）之於高熱製得的二氧化矽爲細粒 白色粉末形式。另一步驟中，於提高溫度下，藉由以含有 水蒸汽的空氣處理，自其中分離仍黏著於二氧化矽上的氫 氯酸殘渣。 摻有銀的火成二氧化矽之BET表面積是206平方米/克 〇 製備條件列於附表1，所得二氧化矽的其他分析數據列 於附表2。 (請先閲讀背面之注意事項
本買)'
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本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） 524774 A7 B7 五、發明説明（5 ) 附表1 製備摻有銀（氧化物）的火成二氧化矽之實驗條件
SiCU 主要空氣 次要空氣 H2核心 H2護套 鹽溶液 氣溶膠量 空氣氣溶膠 BET 公斤/ 立方米/小時 立方米/ 立方米/ 立方米/ 公斤/小 立方米/小 平方米 小時 小時 小時 小時 時 時 /克 4.44 7.5 12 3 0.5 5%Ag2S〇4 水溶液 0.725 0.5 206 註：主要空氣=中央管中的空氣量；H2核心=中央管中的氫 ;氣溶膠量=轉化成氣溶膠形式的鹽溶液的質流速率；空氣 氣溶膠=氣溶膠的載氣（空氣）量；
(請先閱讀背面之注意事項^^寫本頁V 1裝· 寫本 訂 附表2 分析數據 BET pH値 塡塞密度 Ag2〇含量 平方米/克 4 %水性懸浮液 克/升 重量％ 實例 206 4.13 24 1.72 根據本發明之二氧化矽的優點：根據本發明之二氧化 矽具有殺菌性。 主要元件對照表 1 燃燒器
經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐） -8 - 524774 A7 B7 五、發明説明（6 ) 2 中央管 3 噴嘴 4 噴嘴 5 軸管 6 氣溶膠產生器 7 加熱區 (請先閱讀背面之注意事項 本頁)· 訂
經濟部智慧財產局員工消費合作社印製 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -9 -

Claims (1)

1% 524274-- 公告本 A8 B8 C8 D8 iL·-- 、申請專利範圍 附件1 a 第8.9118153號專利申請案 中文申請專利範圍修正本 民國9 1年8月16日修正 1.一種摻有銀或氧化銀之於高溫製得的二氧化矽， 其特點在於：基礎組份是.以火燄氧化或火燄水解方式於高 熱下製得的二氧化矽，此二氧化矽摻有1 X 1 0 _ 4重量 %至2 0重量％的摻雜組份，摻雜組份是銀的鹽或鹽混合 物或銀化合物或金屬銀之懸浮液或它們的混合物，經摻雜 的氧化物之BET表面積爲1至6 00平方米/克。 2 .如申請專利範圍第1項之摻有銀或氧化銀之於高 溫製得的二氧化矽，其中該基礎組份是以火燄水解方式於 高熱下製得的二氧化矽。 3 .如申請專利範圍第1項之摻有銀或氧化銀之於高 溫製得的二氧化矽，其中摻雜量範圍爲1至1 0，0 0 0 p p m 〇 4 .如申請專利範圍第1項之摻有銀或氧化銀之於高 溫製得的二氧化矽，其中經摻雜的氧化物之B E T表面積 爲40至400 平方米/克。 5 · —種製備摻有銀或氧化銀·之火成氧化物的方法， 其特徵在於：將氣溶膠送入用以藉火燄氧化或火燄水解方 式製備火成二氧化矽的火燄中，在反應之前，此氣溶膠與 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） (請先閎讀背面之注意事項再填寫本頁) Γ 經濟部智慧財產局員工消費合作社印製 之， ， 式 合方 混知 勻已 均以 物， 合應 混反 體中 氣錄 的火 應在 反物 解合 水混 燄體 火氣 或 / 應膠 反溶 化氣 氧使 談， 火後 524774 A8 B8 C8 D8 六、申請專利範圍 自氣流中分離所得之摻有銀或氧化銀之火成二氧化矽，以 含有銀的鹽類或鹽混合物的鹽溶液或處於溶解或懸浮形式 的銀金屬或它們的混合物作爲氣溶膠起始物，此氣溶膠可 藉二組份噴嘴以霧化方式或藉其他產製氣溶膠的方法製得 0 6 ·如申請專利範圍第5項之方法，其中該氣溶膠是 利用热溶膠產生器以超音波霧化的方式製得。 7 . —種殺菌塡料，其係由申請專利範圍第1項之藉 热溶膠慘雜銀或氧化銀的火成二氧化砂所組成。 8 ·如申請專利範圍第7項之殺菌塡料，係用於塗漆 與塗料的製造和紙業。 ---------參------1T------0 (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財產局員工消費合作社印製 I錄 準 標 家 國 國 中 用 I適
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