TW574057B - Treating agent for exhaust gas containing metal hydride, process for producing the same, and method of treating exhaust gas containing metal hydride - Google Patents
Treating agent for exhaust gas containing metal hydride, process for producing the same, and method of treating exhaust gas containing metal hydride Download PDFInfo
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經濟部智慧財產万員工消費合作社印製 574057 Α7 Β7 五、發明説明（1 ) 技術領域 本發明係有關含有金屬氫化物之廢氣處理劑及其製造 方法以及含有金屬氫化物之廢氣處理方法。更具體而言係 有關半導體製造步驟發生的含有金屬氫化物之廢氣處理劑 及其製造方法以及其廢氣處理方法。 背景技術 在半導體製造工廠，其製造中使用著各種金屬氫化物 ，鹵化物氣體類。此等氣體由於具有可燃性及/或有毒性 ，在環境保護上，不可將含有此等的廢氣原狀的排放至大 氣中，爲減少其危險性，有害性而採的處理係必需的。 廢氣處理方法係有濕式法及乾式法，前者係以藥液淸 洗處理廢氣之方法，另一方面後者則使廢氣流通於粒狀固 體處理劑之辑充塔內’藉由除害對象氣體及處理劑間之化 學作用，亦即吸附及/或化學反應，分離，除害危險性， 有害性氣體之方法，大多以含有金屬氫化物之廢氣或含有 鹵化物氣體之處理進行著。 至於粒狀固體處理劑，係以已載持金屬鹽於載體上者 ’或將金屬氧化物，金屬氫氧化物或金屬碳酸鹽類成形成 粒狀者被使用著，至目前爲止有多數的金屬成分被揭示著 —「然而此—等ΊΤ氣處理_劑對含有 理能力，因係起因於處理劑及含有金屬氫化物之氣體間之 化學作用，故並非永久固定的。因此，在實際的使用，乃 講求事先可檢測處理性能降低的事情之手段，在該性能喪 本纸張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐） Γ4Ί~~ (請先閲讀背面之注意事項再填寫本頁)Printed by the Intellectual Property of the Ministry of Economic Affairs, 10,000 employees, Consumer Cooperatives 574057 Α7 B7 V. Description of the Invention (1) Technical Field The present invention relates to an exhaust gas treatment agent containing a metal hydride, a manufacturing method thereof, and an exhaust gas treatment method containing a metal hydride. More specifically, the present invention relates to a metal hydride-containing exhaust gas treating agent produced in a semiconductor manufacturing step, a method for manufacturing the same, and an exhaust gas treating method therefor. BACKGROUND ART In a semiconductor manufacturing plant, various metal hydrides and halide gases are used in the manufacture. Because these gases are flammable and / or toxic, in terms of environmental protection, the exhaust gas containing these gases must not be discharged into the atmosphere as they are. Treatments required to reduce their danger and harmfulness are necessary. Exhaust gas treatment methods include wet method and dry method. The former is a method of treating the exhaust gas with a chemical solution, while the latter allows the exhaust gas to circulate in the collection tower of the granular solid treatment agent. And the chemical action between the treatment agents, that is, adsorption and / or chemical reaction, separation, elimination of hazardous, harmful gases, methods are mostly carried out with waste gas containing metal hydride or treatment containing halide gas. As for the granular solid treatment agent, those which have been supported with a metal salt on a carrier or those formed by forming a metal oxide, a metal hydroxide, or a metal carbonate into a granule are used. Until now, most metals have been used. The ingredients are revealed— "However," such gas-treating agents are not capable of permanent fixation because they are due to the chemical action between the treating agent and the gas containing metal hydride. Therefore, in actual use It is a means to detect the degradation of the processing performance in advance. The paper size applies the Chinese National Standard (CNS) Α4 specification (210X297 mm) Γ4Ί ~~ (Please read the precautions on the back before filling in this page)
574057 A7 B7 經濟部智慧財音局員工消費合作社印製 五、 發明説明 (2 ) 失 之 刖 與 新 處 理 劑 交 換 的 方 法 5 或 使 廢 氣 流 通 於 另 外 準 備 的 處 理 劑 塡 充 塔 可 相 互 轉 換 多 數 的 處 理 劑 塡 充 塔 而 使 用 的 方 法即 成 爲 必 要 的 〇 於 含 有 金 屬 氫 化 物 之 廢 氣 處 理 劑 方 面 發 現 有 多 件 專 利 3 例 如 由 金 屬 氫 氧 化 物 5 金 屬 碳 酸 鹽 或 鹼 性 金 屬 碳 酸 鹽 而 成 的 處 理 劑 5 係 如 曰 本 特 開 平 〇 5 — 2 8 4 8 4 7 號 曰 本 特 開 平 〇 6 — 3 1 9 9 4 5 號 5 曰 本 特 開 平 〇 8 — 1 9 2 〇 2 4 號 5 曰 本 特 公 平 〇 5 — 6 1 9 6 6 號 5 註 冊 專 利 第 2 6 〇 4 9 9 1號公報等所示般。 此 等 專 利 中 揭 示 的 處 理 劑 可 使 用 市 售 的 金 屬 氫 氧 化 物 作 爲 金 屬 化 合 物 或 利 用 金 屬 鹽 類 及 氫 氧 化 驗 之 中 和 反 "匕、 而 得 的 金 屬 氫 氧 化 物 或使 用 市 售 的 金 屬 碳 酸 鹽 類 作 爲 .金 屬 化 合 物 3 或 利 用 金 屬 鹽 類 及 驗 碳 酸 鹽 類 之 中和 反 應 而 得 的 金 屬 驗 性 碳 酸 鹽 〇 此 等 金 屬 化 合 物 類 係 可 予 單 獨 使 用. 爲 改 善 金 屬 化 合 物 之 物 理 或 化 學 性 狀 可 組 合 氧 化 鎂 7 二 氧 化 矽 3 重 金 屬 化 合 物 類 3 二 氧 化 欽 5 驗 石 灰 等 多 種 無 機 化合 物 類 而' 予使用 〇 .例 如 於 曰 本 註 冊 專 利 第 2 9 2 6 4 5 9 號 公 報 內 ， 揭 示 有 於 藉 由 市 售 的 氫 氧 化 銅 或 銅 鹽 與 氫 氧 化 鉀 之 中 和 反 應 而 得 的 氫 氧 化 銅 內 5 已 添 加 各 種 金 屬 化 合 物 作 爲 安 定 化 劑 之 處 理 劑 ，係作爲由金屬氫氧化物 1而 成 的 處 理 劑 0 於 曰 本 特 公 平 5 — 6 1 9 6 6 號 公 報 中 5 揭 示 有 使 用 金 屬 化 合 物 之 鹼 性 碳 酸 銅 的 處 理 劑 〇 該 處 理 劑 係 將 藉 由 銅 m ΓΓΠ- 類 及 碳 酸 驗 之 中 和 製 備 的 驗 性 碳 酸 銅 以 乾 式 或 濕 式 方 (請先閱讀背面之注意事項再填寫本頁) 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -5 - 、11 經濟部智慧財矣局員工消費合作社印製 574057 A7 _ B7 五、發明説明（3 ) 式塗布於鹼石灰上而予製造。 於3主冊專利第2 6 0 4 9 9 1號公報中，同樣的揭不 有使用金屬化合物之鹼性碳酸銅的處理劑。此處理劑係將 ’以銅鹽類水溶液及碳酸鈉水溶液之中和反應而得的鹼性碳 酸銅與銳鈦礦型二氧化鈦濕式混練後，予以成型而製造的 。且該鹼性碳酸銅係p Η値由中性至弱鹼性狀態使生成沈 澱’分子式表示成CuC〇3· Cu (0Η) 2時，於所得 的化合物中含有的〇Η基量係成爲其1 · 1倍以上的化合 物。 . 又於曰本特開平8 - 1 9 2 0 2 4號公報中，揭示有 金屬碳酸鹽或金屬鹼性碳酸鹽係由Cu，Ζη，Μη， F e ’ C ο ，N i而成的群體選擇的至少一種以上之金屬 碳酸鹽或金屬鹼性碳酸鹽而成，此等金屬碳酸鹽或金屬鹼 性碳酸鹽雖可以試藥或工業藥品購得，但由對應的金屬鹽 類水溶液依常法製造者，已成形該金屬碳酸鹽或該金屬鹽 驗性碳酸鹽之處理劑。 再者，於日本特開平1 〇 - 23 5 1 85號公報，日 本特開平1 1 一 0 1 9 4 7 5號公報等，.揭示有由金屬氧 化物而成的處理劑。以由二種以上的金屬氧化物，具體而 言指氧化銅，氧化銀，二氧化錳之中選擇的氧化物爲主成 分常濃度之金屬氣crrnii之勝 氣的處理劑。 且於上述公報內，此等金屬化合物爲氫氧化物或碳酸 鹽類時，由於藉由除害氣體之吸附及/或與除害氣體間之 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -6 - 一 ？ · 1 - I I I— 11^1 ·ί : ; In I- I - -..... m·^、一I-— nn 1 - —1 - - (請先閱讀背面之注意事項再填寫本頁) 經濟部智慧財音局員工消費合作社印製 574057 A7 _B7__ 五、發明説明（4 ) 化學反應而變色，藉由目視’監視處理劑色調變化’可檢 測處理劑之殘存除害性能’加上用作處理劑之作用’即使 用作金屬氫化物氣體洩漏之檢測劑亦有用一事亦經予揭示 著。 利用金屬化合物類之含有金屬氫化物之廢氣之處理’ 係歸因於處理劑及除害對象氣體間之吸附及/或化學反應 ，故爲提高處理劑之金屬氫化物氣體處理能力’以提高上 述吸附性，吸附容量’反應性等係有效的。然而’由上述 的金屬氫氧化物，金屬碳酸鹽或金屬鹼性碳酸鹽而成之習 用技術之處理劑’係對一般的工業製品或沈殿法而得的化 合物類原狀的成型並予使用，或與另外的化合物類混合後 成型而僅予使用，故再殘存著可提高性能之創意工夫的餘 又，伴隨上述廢氣之處理的化學反應不論何者係發熱 性。因此利用金屬化合物類之廢氣處理必然會有溫度上升 現象，進行含有高濃度之金屬氫化物之廢氣處理或大量的 廢氣處理時，有生成大幅的溫度上升之可能性。因此，不 僅處理劑係高性能，亦被要求需具低發熱性。 尤其，對廢氣含有氫時，由於伴隨處理而發生的熱之 累積，使處理劑層之溫度上升，有引起利用氫之處理劑金 原反應的可能性，此還原反 更可助長溫度上升，有加上處理劑金屬成分之物理性狀的 變質’或劣化對廢氣處理裝置材質有惡劣影響的顧慮。因 此，廢氣含有氫氣之情形，處理劑係被要求不僅除害性能 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） TjZ ' --- (請先閱讀背面之注意事項再填寫本頁)574057 A7 B7 Printed by the Consumer Cooperatives of the Smart Finance and Sound Bureau of the Ministry of Economic Affairs 5. Description of the invention (2) Method 5 for exchange of lost fuel with a new treatment agent 5 Or the exhaust gas can be circulated to a separately prepared treatment agent The method of filling the treatment agent with the tower becomes necessary. Several patents have been found in the exhaust gas treatment agent containing metal hydride. 3 For example, treatment with metal hydroxide 5 metal carbonate or alkaline metal carbonate. Agent 5 is as described in Japanese Patent Publication No. 05-2 8 4 8 4 7 Japanese version of Japanese Patent Publication No. 6-3 1 9 9 4 5 No. 5 Japanese version of Japanese Patent Publication No. 8-1 9 2 0 2 4 Special fair 0-5 6 1 9 6 6 Registered patent No. 2 0 4 9 9 1 and the like. The treatment agents disclosed in these patents can use commercially available metal hydroxides as metal compounds or use metal salts and hydroxides to neutralize the reaction " metal hydroxides or use commercially available metals Carbonates are used as metal compounds 3. Or metal carbonates obtained by neutralization of metal salts and carbonates. These metal compounds can be used alone. To improve the physical or chemical properties of metal compounds It can be used in combination with magnesium oxide, 7 silicon dioxide, 3 heavy metal compounds, 3 calcium dioxide, and 5 kinds of inorganic compounds such as lime. For example, in Japanese Patent Registration No. 2 9 2 6 4 5 9 Various metal compounds have been added to copper hydroxide obtained by neutralization reaction of commercially available copper hydroxide or copper salt with potassium hydroxide. The stabilizer is a treatment agent composed of a metal hydroxide 1. As described in Japanese Patent Publication No. 5-6 1 9 6 6, a treatment agent using a basic copper carbonate containing a metal compound is disclosed. 〇This treatment agent will be prepared by copper m ΓΓΠ- and carbonic acid test neutral copper carbonate dry or wet (please read the precautions on the back before filling this page) This paper size applies to China Standard (CNS) A4 specification (210X 297 mm) -5-、 11 Printed by the Consumer Cooperatives of the Ministry of Economy and Finance Bureau 574057 A7 _ B7 V. Description of the invention (3) It is coated on soda lime and manufactured. In the 3 main book patent No. 2 0 4 9 91, the same is not disclosed as a treatment agent for a basic copper carbonate using a metal compound. This treatment agent is prepared by wet-kneading alkaline copper carbonate and anatase-type titanium dioxide obtained by neutralizing a copper salt-based aqueous solution and a sodium carbonate aqueous solution, and then molding. In addition, when the basic copper carbonate-based p Η 値 is precipitated from a neutral to weakly basic state, and the molecular formula is expressed as CuC0 · Cu (0Η) 2, the amount of the Η group contained in the obtained compound becomes 1 · 1 times more compounds. In Japanese Patent Application Laid-Open No. 8-1 920 0 2, it is disclosed that a metal carbonate or a metal basic carbonate is a group consisting of Cu, Zn, Mn, Fe'C, and Ni. It is made by selecting at least one or more metal carbonates or metal basic carbonates. Although these metal carbonates or metal basic carbonates can be purchased in trials or industrial medicines, they are prepared from the corresponding metal salt aqueous solution according to the usual method. The manufacturer has formed the treatment agent for the metal carbonate or the metal salt test carbonate. In addition, in Japanese Patent Application Laid-Open No. 10-23 5 1 85, Japanese Patent Application Laid-Open No. 1 1 0 1 9 45, etc., there are disclosed treatment agents made of metal oxides. The treating agent for metal gas crrnii, which is composed of two or more kinds of metal oxides, specifically, copper oxide, silver oxide, and manganese dioxide, is used as the main component. And in the above bulletin, when these metal compounds are hydroxides or carbonates, because of the adsorption and / or detoxification of the paper on the paper size, the Chinese National Standard (CNS) A4 specification ( 210X297 mm) -6-One? · 1-III— 11 ^ 1 · ί:; In I- I--..... m · ^ 、 一 I-— nn 1-—1--(Please read the notes on the back before filling this page ) Printed by the Consumer Finance Cooperative of the Ministry of Economic Affairs and the Ministry of Economic Affairs, Consumer Cooperative 574057 A7 _B7__ V. Description of the Invention (4) Discoloration due to chemical reaction, by visual inspection of 'Monitoring the change in color of the treatment agent', the residual damage removal performance of the treatment agent can be detected ' As a treatment agent, it has been revealed that it is useful even as a detection agent for metal hydride gas leakage. The treatment of waste gas containing metal hydrides using metal compounds is due to the adsorption and / or chemical reaction between the treatment agent and the gas to be harmed, so to improve the metal hydride gas treatment capacity of the treatment agent to improve the above Adsorption, adsorption capacity, and reactivity are effective. However, the "treatment agent for conventional technology made of the above-mentioned metal hydroxide, metal carbonate or metal basic carbonate" is a general industrial product or a compound obtained by the Shen Dian method, and is used as it is, or It is mixed with other compounds to be molded and used only, so there is still room for creative efforts to improve performance, and the chemical reaction accompanying the treatment of the exhaust gas is exothermic. Therefore, the treatment of waste gas using metal compounds will inevitably cause a temperature rise. When a waste gas treatment containing a high concentration of metal hydride or a large amount of waste gas treatment is performed, there is a possibility that a large temperature rise may be generated. Therefore, not only the treatment agent is high-performance, but also requires low heat generation. In particular, when the exhaust gas contains hydrogen, the temperature of the treatment agent layer rises due to the accumulation of heat that accompanies the treatment, which may cause the reaction of the gold agent using the hydrogen treatment agent. This reduction can even promote the temperature rise. There is a concern that the physical properties of the metal components of the upper treatment agent are deteriorated or deteriorated, which has a bad influence on the material of the exhaust gas treatment device. Therefore, in the case that the exhaust gas contains hydrogen, the treatment agent is required to not only harm the performance. This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) TjZ '--- (Please read the precautions on the back before filling this page)
、1T 574057, 1T 574057
A7 B7 經濟部智慧財喜局員工消費合作社印製 五、 發明説明 (5 尚 且 需 爲 低 發 埶 Μ NN 丨生 0 發 明 之 揭 示 含 有 金 屬 氫 化 物 之 廢 氣 處 理 劑 之 除 害 作 用 係起 因 於 處 理 劑 與 含有 金 屬 氫 化 物 之 廢 氣 間 之 吸 附 性 及 / 或 反 性 5 故 可 被 預 測 爲 使 處 理 劑 中 的 有 效 成 分 之 結 晶 子 直 徑 微 細 化 以 增 大 其 表 面 積 可 提 高 除 害 作 用 之 性 能 〇 妖 J \ \\ 而 3 以 公 知 的 處 理 劑 使 用 的 金 屬 化 合 物 類 原 料 係 藉 由 市 的 金 屬 氫 氧 化 物 鹼 性 金 屬 碳 酸 鹽 5 或 其 鹽 類 與 驗 性 化 合 物 間 之 中 和 反 Jffi 予 以 製 造 的 金 屬 化合 物 類 可 被 視 作 不 —^ 定 爲 具 有 符 合 g 的 之 物 理 性狀之原料£ > 又 於 藉 由 其 鹽 與 驗 性 化 合 物 間 之 中 和 反 應 製 造 金 屬 化 合 物 時 ， 所 得 的 沈 澱 物 係 在 其 後 ? 經 cm 過 熟 成 ， 水洗 > 過 濾 > 乾 燥 等 的 步 驟 以 至 兀 成 惟 其 中 用 作 沈 澱 劑 之 鹼 性 化 合 物 之 種 類 ， 中 和 反 應 條 件 乾 燥 條 件 等 最 終 可 得 的 金 屬 化 合 物 之 結 晶' 子1 直徑 ，表面積係受影響。 本 發 明 人 等 對 用 作 含 有 金 屬 氫 化 物 之 廢 氣 處 理 劑 之 提 局 性 能 方 法 5 藉 由 深 入 探 究 其 製 造 條 件 改 善 有 效 金 屬 成 分 之 物 性 經 桐 心 檢 討 未 能 達 成 性 能 提 筒 之 同 時 對 藉 由 添 加 構 安 定 化 物 質 於 金 屬 化 合 物 內 的 微 結 晶 子 化 局 表 面 積 化 進 行 檢 討 〇 至 於化 合 物 之 構 造 安 定 化 物 已 知 有 二 氧 化 矽 y 氧 化 鋁 ， 氧 化 鎂 二 氧 化 鈦 5 氧 化 Wu 等 惟 僅 以 單 單 混 合 添 加 此 等 物 質 於 金 屬 化 合 物 內 7 可 使 其 微 結 晶 子 化 ， 高 表 面 積 化 效 果 減 少 0 再 者 ， 採 用 以 已 懸 浮 此 等 物 質 穿裝-- (請先閱讀背面之注意事項再填寫本頁) 、1T Φ 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -8 - 574057 (請先閱讀背面之注意事項再填寫本頁)A7 B7 Printed by the Consumer Finance Cooperative Bureau of the Ministry of Economic Affairs of the Wealth and Wealth Bureau. 5. Description of the invention (5 still needs to be low-intensity 埶 NN 丨 Health 0 The disclosure of the invention reveals that the harmful effect of the waste gas treatment agent containing metal hydride is caused by the treatment agent Adsorption and / or reactivity with exhaust gas containing metal hydride5 Therefore, it can be predicted that the crystal diameter of the active ingredient in the treatment agent can be miniaturized to increase its surface area to improve the performance of detoxification. \ \\ And 3 metal compound raw materials used in known processing agents are metal compounds produced by neutralizing anti-Jffi between metal hydroxides, basic metal carbonates 5 or their salts and test compounds. The class can be regarded as not-^ determined as a raw material with physical properties conforming to g > between the salt and the test compound When the metal compound is produced by the neutralization reaction, the resulting precipitate is followed by the steps of over-maturation in cm, washing with water, filtration, drying, and the like to form only the basic compounds used as precipitants in the medium. The diameter and surface area of the crystals of the metal compound finally available, such as drying conditions and reaction conditions, are affected. The present inventors' method for improving the performance of a metal hydride-containing exhaust gas treatment method 5 By further exploring its Manufacturing conditions improve the physical properties of effective metal components. After reviewing Tongxin's failure to achieve the performance improvement, the microcrystallized localized surface area of the metal compound by the addition of a stabilizing substance was reviewed. As for the structural stability of the compound, It is known that silica, alumina, magnesia, titania, 5 and Wu, etc. are only added by mixing Adding these substances to the metal compound 7 can make them crystallize and reduce the effect of high surface area. Furthermore, they should be worn with these substances suspended (Please read the precautions on the back before filling this page) 、 1T Φ This paper size is applicable to China National Standard (CNS) A4 specification (210X297mm) -8-574057 (Please read the precautions on the back before filling this page)
A7 B7 經濟部智慧財A局員工消費合作社印製 五、 發明説明 (6 ) 之 金 屬 鹽 類 水 溶 液 爲 沈 澱 母 液 5 進 行 沈 澱 操 作 ， 即 使 添 加 於 金 屬 化 合 物 中 仍 然 亦 使 其 微 結 晶 子 化 5 高 表 面 積 化 效 果 變 小 〇 在 此 再 進 行 金 屬 化 合 物 之 物 性 改 善 中 並 非 以 構 造 安 定 化 物 爲 粉 末 添 加 入 沈 澱 母 液 嘗 試 藉 由 使 與 有 效 金 屬 成 分 共 沈 降 的 添 加 〇 利 用 金 屬 化 合 物 類 之 含 有 金 屬 氫 化 物 之 處 理 係 由 開 始 後 之 吸 附 作 用 及 / 或 化 學 反 應 ， 經 CIH, 過 時 間 使 處 理 劑 溫 度 上 升 後 3 移 行 至 化 學 反 應 ， 化 學 反 應 爲 中 心 的 固 定 的 除 害 過 程 係 消 耗 大 部 分 的 金 屬 成 分 爲 止 予 以 繼 續 關 於 金 屬 成 分 之 化 學 的 形 態 及 發 熱 性 以 金 屬 氫 氧 化 物 金 屬 碳 酸 鹽 ， 金 屬 鹼 性 碳 酸 鹽 較 氧 化 物 在 固 定 的 除 害 過 程 可 被 視 作 低 發 熱 性 5 故 使 與 上 述 構 造 安 定 化 劑 共 沈 . 降 的 沈 澱 物 ， 止 於 僅 乾 燥 最 終 處 理 重 複 各 種 試 誤 並 檢 討 其 效 果 〇 亦 即 採 用 氫 氧 化 鉀 驗 碳 酸 鹽 爲 沈 澱 劑 ， 添 加 溶 解 鹼 矽 酸 鹽 於 其 中 ， 其 次 藉 由 使 用 沈 澱 劑 進 行 與 金 屬 鹽 間 之 中 和 反 應 於 使 金 屬 成 分 及 矽 成 分 共 沈 降 時 3 所 得 的 沈 澱 物 係 由 此 等 成 分 化 合 物 之 混 合 物 或 此 等 成 分 化 合 物 之 一 部 分 已 形 成 複 合 體 之 混 合 物 而 成 可 得 知 金 屬 成 分 係 局 分 散 化 5 具 有 局 表 面 積 〇 至 於 此 混 合 物 ， 在 進 行 金 屬 氫 化 物 氣 體 之 除 害 性 測. 定 試 驗 時 亦 較 由 金 屬 氧 化 物 而 成 的 處 理 劑 使 發 熱 引 起 的 溫 度 上 升 小 5 而 且 確 認 出 高 性 能 以 至 完 成 本 發 明 〇 本 發 明 係 關 於 藉 由 銅 鹽 類 水 溶 液 及 含 有 鹼 矽 酸 鹽 類 本紙張尺度適用中國國家標準（CNS ) A4規格（210X 297公釐） -9 - 574057 A7 B7 五、發明説明（7 ) 之氫氧化鹼，鹼碳酸鹽或鹼重碳酸鹽類水溶液間之中和反 應予以製造的氫氧化銅或鹼性碳酸銅與矽化合物混合的混 合物，或（形成）前述氫氧化銅或前述鹼性碳酸銅之一部 分爲矽化合物與複合體之混合物，前述混合物之c u / S i之原子比爲1〜1 0之含有金屬氫化物之廢氣處理劑 及其製造方法與其含有金屬氫化物之廢氣處理方法者。 本發明使用的銅鹽類，若爲硝酸鹽，硫酸鹽，氯化物 ，有機酸鹽類等，水溶性鹽類時，則不論任何鹽類亦可使 用。且，在本發明係使用該銅鹽類之水溶液（A液）作爲 沈源母液。 經予使用作沈澱劑之化合物，係以氫氧化鹼，鹼碳酸 鹽或鹼重碳酸鹽，使用鈉或鉀作爲鹼，至於鹼矽酸鹽係以 Na2〇· nS i〇2 · nH2〇 （n = 2〜4)之化學式 表示的石夕酸鈉，K2〇· nS i〇2 · nH2〇 （n = 3〜 4 )表不的政酸鉀爲宜，於氫氧化鹼，驗碳酸鹽或鹼重碳 酸鹽之水溶液內添加鹼矽酸鹽並已溶解的混合水溶液則被 使用作沈澱劑（B液）。 C u及S i之含有量，若以C u/S i之原子比表示 時’則在1〜1 0之範圍，其原子比較1小時，大部分的 銅化合物形成矽化合物及複合體係由X -射線繞射之構造 以確認，與金屬氫化物氣體簡的游離 之銅化合物含有量會變少，故處理劑之除害容量變小，故 並不宜。又其原子比較1 〇大時，未能得由已微細化的銅 化合物而成的高表面積之處理劑，並非用作處理劑之較宜 本紙張尺度適用中國國家標準（CNS ) A4規格（21〇X297公釐) ~1〇 - " (請先閱讀背面之注意事項再填寫本頁) 、\一一口 Φ 經濟部智慧財-4局員工消費合作社印製 574057 A7 B7 ^ 五、 發明説明 (8 ) I j 的 物 性 0 1 I 在 沈 澱 操 作 方 面 5 於 A 液 添 加 Β 液 之 正 中 和 ， 於 B 液 1 1 添 加 A 液 之 逆 中 和 或 於 經 予 準 備 的 沈 澱 劑 內 加 水 並 於 其 产^S 请 1 中 同 時 添 加 A B 兩 液 的 一 定 P Η 下 之 中 和 等 〇 即 使 藉 由 先 閱 1 任 操 作 亦 可 使 生 成 良 好 的 沈 澱 ， 惟 將 於 此 操 作 之 終 點 背 面 I | 的 Ρ Η 値 設 成 中 性 弱 驗 性 係 重 要 的 P Η 値 若 由 此 範 圍 之 意 1 -·» I 超 出 時 則 未 能 獲 得 由 較 宜 的 物 性 之 銅 化 合 物 而 成 的 處 理. 事 項 再 填 % 劑 〇 寫 本 裝 | 由 中 和 反 應 而 得 的 沈 澱 物 係 在 熟 成 後 經 予 水 洗 乾 頁 1 1 燥 ό 在 此 水 洗 係 去 除 混 雜 於 沈 澱 物 中 的 驗 化 合 物 ， 所 得 • 的 處 理 劑 之 物 性 係 在 後 步 驟 爲 抑 制 變 質 而 予 進 行 於 最 後 1 I 所 得 的 處 理 劑 中 殘 存 的 驗 量 水 洗 至 0 • 1 % 以 下 爲 止 較 宜 1 訂 I 〇 其 次 進 行 的 乾 燥 係 處 理 劑 化 合 物 不 引 起 埶 J \ \\ 變 質 於 製 造 1 時 間 縮 短 內 合 理 的 溫 度 範 圍 ? 以 在 8 〇 2 0 〇 °C 進 行 爲 1 1 宜 0 溫 度 若 較 8 〇 °c 低 時 乾 燥 時 era, 過 於 耗 費 時 間 5 並 不 實 ! % I .用 〇 若 較 2 〇 〇 °C 商 時 則 氫 氧 化 銅 鹼 性 碳 酸 銅 之 一 部 分 分 解 會 生 成 里 / \ w 色 的 氧 化 銅 故 實 用 上 欲 藉 由 處 理 劑 之 1 1 1 經 變 色 而 確 認 處 理 劑 之 殘 存 除 害 性 能 一 事 係. 有 困 難 同 時 會 1 濟 部 使 除 害 性 能 降 低 0 再 者 在 已 含 有 氫 之 含 有 金 屬 氫 化 物 之 廢 1 慧 貝才 _^ 氣 處 理 的 發: 熱: 量變成尤其大。 1 局 員 所 得 的 乾. 燥 物 係 呈 ΓΤΠ. 綠 色 具 有 氫 氧 化 銅 或 鹼 性 碳 酸 1 I 工 消 銅 及 結 晶 水 之 二 氧 化 矽 的 混 合 物 或 此 等 化 合 物 之 一 部 分 1 Κ 合 形 成 複 合 體 的; 混合物 。此混合物係由 丨乳 丨用 氮 吸 附而 求 的 1 1 社 印 製 Β Ε Τ 表 面 積 爲 1 〇 〇: m : 1 / 'g 以 、上， X —— 射 線 繞 射 之 銅 化 1 ! 1 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -11 - 574057 A7 B7 五、發明説明（9 ) (請先閱讀背面之注意事項再填寫本頁) 合物’亦即氫氧化銅或鹼性碳酸銅之結晶子直徑爲 5 0 n m以下的微細結晶而成，表面積較1 m 2 / g少 時，未能獲得表示高性能之處理劑，銅化合物之結晶子直 徑較5 0 n m大時亦由於銅之分散性不足而未能獲得表示 尚性能之處理劑。此事係藉由表示出處理劑中之鹼性碳酸 銅結晶子直徑及用作金屬氫化物氣體之矽烷氣體除害性能 之關係圖1 ，可顯而得知，且鹼性碳酸銅之結晶子直徑愈 小時除害性能愈高。此關係在氫氧化銅之結晶子直徑及金 屬氫化物氣體除害性能亦係相同的。 本發明之金屬化合物，係於使用氫氧化鹼作爲沈澱劑 時，由氫氧化銅及矽系化合物而成的混合物或氫氧化銅及 矽化合物之部分形成複合體之混合物。以鹼碳酸鹽或鹼重 碳酸鹽爲沈澱劑時爲鹼性碳酸銅及矽化合物之混合物或此 等化合物之一部分形成複合體之混合物。至於鹼性碳酸銅 ’爲以 CuC〇3· 2Cu (〇H)2，3CuC〇3· 經濟部智慧財A局員工消費合作社印製 5 C u (OH) 2-H2〇 ^ CuCOs· Cu (〇H)2, CuC〇3.Cu (〇Η)2·Η2〇等表示的化合物類之 混合物，於與銅鹽類水溶液之中和反應，使用鹼碳酸鹽， 或鹼重碳酸鹽類水溶液時，用作碳酸根之二氧化碳氣體（ C〇2)含有量對全部重量宜爲5%以上，其量較5%少時 ，部分成爲氧化物化物之^廢氣處發起-性大，除害性能會變低。 其次，說明本發明之處理方法。將藉由含有銅鹽水溶 液及矽酸鹼之氫氧化鹼，鹼碳酸鹽或鹼重碳酸鹽類水溶液 -12- 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） 574057 Α7 Β7 五、發明説明（) ▼裝-- (請先閱讀背面之注意事項再填寫本頁) 之中和反應而得的沈澱物予以熟成，水洗，乾燥而得的乾 燥物予以擠壓，打成錠片，製造成成型物的本發明之處理 劑，塡充於流動式塡充塔內，其次藉由使含有金屬氫化物 之還原性廢氣接觸，可將金屬氫化物予以除害。 至於可由本發明處理劑除害的金屬氫化物氣體類，有 矽烷，胂，膦，二矽烷，二硼烷，硒化合物，鍺，二氯矽 烷等。本發明處理劑因係以氫氧化銅或鹼性碳酸銅爲主體 ，故呈現藍綠色，藉由與此等金屬氫化物氣體類間之接觸 而成的吸附及/或化學反應會變色，具有可探究由目視， 觀察該色調變化狀況殘存的處理性能之優點。 ·# 本發明人等係將藉由系列的操作製造的本發明之處理 劑塡充於不銹鋼製流動式反應器內，使含有金屬氫化物氣 體之矽烷或膦之還原性氣體流入反應器內，同時·進行處理 劑層之溫度測定，同時藉Brack mοnitor (Biοnix公司製造）測 定出口氣體中的金屬氫化物氣體洩漏量，並予監視，進行 於常溫之含有金屬氫化物之氣體的除害性能測定試驗。 經濟部智慧財甚局員工消費合作社印製 結果經長期間於出口氣體中並未予檢測出金屬氫化物 ，其除害性能（L / 1 〇 g )係以共沈降以外的方法添加 的處理劑較由公知的同種金屬化合物而成的處理劑，亦即 僅有效金屬成分之處理劑，或構造安定化劑有高性能，故 本處理齒if確認出具有優越的金屬氫 且於以氧化物系處理劑實施相同的試驗時，在開始試 驗後，由於處理劑層在不正常反應的溫度上升顯著，對繼 續性能測定試驗係困難的，而本發明處理劑之情形雖可被 本紙張尺度適用中國國家標準（CNS ) Α4規格（210Χ29?公釐） 「13 - ' 574057A7 B7 Printed by Employees ’Cooperatives of the Bureau of Wisdom and Finance of the Ministry of Economic Affairs. 5. Description of the invention (6) The metal salt aqueous solution is the precipitation mother liquor. 5 Precipitation operation, even if it is added to metal compounds, it still crystallizes 5 High surface area The chemical conversion effect is reduced. In this case, the physical properties of the metal compound are not improved, and the structural mother compound is not added as a powder to the precipitation mother liquor. The addition is attempted by co-sedimentation with an effective metal component. The metal compound-containing metal hydride treatment is used. After the start of the adsorption and / or chemical reaction, after the CIH, the temperature of the treatment agent rises over time. 3 After the transition to the chemical reaction, the fixed detoxification process centered on the chemical reaction is continued until the most metal components are consumed. About the chemical form and exothermicity of metal components It is a hydroxide metal carbonate, metal alkaline carbonate can be regarded as a lower exothermic than the oxide in the fixed detoxification process.5 So co-sedimentation with the above-mentioned structural stabilizers. Reduced precipitates, only to dry The final treatment was repeated various trial and error and its effect was reviewed. That is, potassium hydroxide was used to test the carbonate as a precipitating agent, and a dissolved alkali silicate was added thereto, followed by neutralizing the reaction with the metal salt by using a precipitating agent. When the metal component and the silicon component are co-precipitated, the precipitate obtained is a mixture of these component compounds or a part of these component compounds that have formed a complex. It can be seen that the metal component system is locally dispersed 5 and has a local surface area. As for this mixture, the metal hydride gas is tested for its harmfulness. It is also compared with metal oxygen The treatment agent made of the material reduces the temperature rise caused by heat generation5 and has confirmed the high performance to complete the present invention. The present invention relates to the use of copper salt aqueous solutions and alkali silicates. ) A4 size (210X 297 mm) -9-574057 A7 B7 V. Description of the invention (7) Copper hydroxide or alkali produced by neutralization reaction between alkali hydroxide, alkali carbonate or alkali bicarbonate aqueous solution A mixture of a basic copper carbonate and a silicon compound, or (forming) a part of the aforementioned copper hydroxide or the aforementioned basic copper carbonate is a mixture of a silicon compound and a complex, and the atomic ratio of cu / Si of the aforementioned mixture is 1 to 1 0 A metal hydride-containing exhaust gas treating agent, a method for manufacturing the same, and a metal hydride-containing exhaust gas treating method thereof. The copper salts used in the present invention are nitrates, sulfates, chlorides, organic acid salts, and the like, and water-soluble salts can be used regardless of any salts. In addition, in the present invention, the copper salt-based aqueous solution (liquid A) is used as the sink source mother liquid. Compounds that are used as precipitating agents are alkali hydroxide, alkali carbonate or alkali bicarbonate, and sodium or potassium are used as the base. For alkali silicate, Na2〇 · nS 〇2 · nH2〇 (n = 2 ~ 4) Sodium oxalate represented by the chemical formula, K2〇 · nS i〇2 · nH2〇 (n = 3 ~ 4) is suitable for the acid potassium, which is used in alkali hydroxide, carbonate or alkali test A mixed aqueous solution containing an alkali silicate dissolved in an aqueous solution of a bicarbonate is used as a precipitant (liquid B). The content of Cu and Si, if expressed in the atomic ratio of Cu / Si, is in the range of 1 to 10, and the atoms are compared for 1 hour. Most copper compounds form silicon compounds and the composite system consists of X -The structure of ray diffraction is used to confirm that the content of free copper compounds with the metal hydride gas will be reduced, so the harm-removing capacity of the treatment agent will be small, which is not suitable. When its atomic ratio is 10, it is not possible to obtain a high surface area treatment agent made of a refined copper compound. It is not suitable as a treatment agent. The paper size applies the Chinese National Standard (CNS) A4 specification (21 〇X297mm) ~ 1〇- " (Please read the notes on the back before filling out this page), \ Yi Yikou Φ Printed by the Ministry of Economic Affairs, Smart Finance-4 Bureau employee consumer cooperative 574057 A7 B7 ^ V. Description of the invention (8) Physical properties of I j 0 1 I In Shendian operation 5 Add neutralization of solution B to solution A, and neutralization of solution B to solution 1 1 Add reverse solution of solution A or add water to the prepared precipitant and add Production ^ S Please add AB two fluids at the same time in certain P Η and neutralize etc. 〇 Even by reading 1 operation first, a good precipitation can be generated, but at the end of this operation I | P Η値 It is important to have weak neutrality. P 値 If the meaning of this range is 1-· » Get a treatment made of copper compounds with better physical properties. Fill in the matter again %% agent 0 writing pack | The precipitate obtained by the neutralization reaction is washed with water after drying. Page 1 1 Drying is removed in this washing system The physical properties of the test compound mixed in the precipitate are: • The physical properties of the obtained treatment agent are to be washed in the final step of the treatment agent obtained in the last 1 I in order to suppress deterioration. It is preferable to wash the test agent to 0 • 1% or less. 1 Order I 〇 Next, the drying treatment compound does not cause 埶 J \ \\ deterioration in a reasonable temperature range within a short time to manufacture? 1 at 1 0 0 0 0 ° C if the temperature is higher than 8 〇 ° c When drying at low temperature, it takes too much time 5 is not true!% I. If it is quotient higher than 2000 ° C, a part of copper hydroxide alkaline copper carbonate will be partially decomposed to produce li / \ w color Copper oxide is practically intended to confirm the residual harm removal performance of the treatment agent by discoloration of the treatment agent. 1 1 1 It is difficult to reduce the harm removal performance of the Ministry of Economic Affairs at the same time. Waste of hydride 1 Hui Beicai ^^ Gas treatment: Heat: The amount becomes particularly large. 1 The dried and dried matter obtained by the bureau member is ΓΤΠ. Green is a mixture of copper hydroxide or basic carbonic acid, 1 I, industrial copper and crystalline silicon dioxide, or a part of these compounds. 1 K is combined to form a complex; the mixture . This mixture is produced by 丨 milk 丨 with nitrogen adsorption. The surface area of Β Ε Τ is 100: m: 1 / 'g or more, X —— ray diffraction copperization 1! 1 copies Paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) -11-574057 A7 B7 V. Description of the invention (9) (Please read the precautions on the back before filling this page) The compound 'is copper hydroxide Or the basic copper carbonate has fine crystals with a crystal diameter of 50 nm or less, and the surface area is less than 1 m 2 / g, a high-performance treatment agent cannot be obtained, and the crystal diameter of a copper compound is smaller than 50 nm Da Shi also failed to obtain a treatment agent that exhibited performance due to insufficient copper dispersibility. This is shown in Figure 1 by showing the relationship between the diameter of the basic copper carbonate crystals in the treatment agent and the silane gas detoxification performance of the metal hydride gas. The smaller the diameter, the higher the harmfulness. This relationship is also the same for the crystal diameter of copper hydroxide and the detoxification performance of metal hydride gas. When the metal compound of the present invention uses alkali hydroxide as a precipitant, a mixture of copper hydroxide and a silicon-based compound or a mixture of copper hydroxide and a silicon compound to form a complex. When alkali carbonate or alkali bicarbonate is used as the precipitant, it is a mixture of basic copper carbonate and silicon compounds or a mixture of a part of these compounds to form a complex. As for the basic copper carbonate, 5 Cu (OH) 2-H2, CuCOs, Cu (〇) were printed with CuC03 · 2Cu (〇H) 2, 3CuC〇3 · The Employees' Cooperative of the Bureau of Intellectual Property A of the Ministry of Economic Affairs. H) 2, a mixture of compounds represented by CuC03.Cu (〇Η) 2 · Η20, etc., when neutralized with a copper salt aqueous solution, when an alkali carbonate or an alkali bicarbonate aqueous solution is used, The content of carbon dioxide gas (CO2) used as carbonate should be more than 5% for the total weight, and when the amount is less than 5%, some of them will become oxides. At the exhaust gas, the property will be large, and the harmfulness will change. low. Next, the processing method of the present invention will be described. Will use copper hydroxide solution and alkali silicate alkali hydroxide, alkali carbonate or alkali bicarbonate aqueous solution-12- This paper size applies to Chinese National Standard (CNS) A4 specification (210X297 mm) 574057 Α7 Β7 five 、 Explanation of the invention () ▼ Packing-(Please read the precautions on the back before filling in this page) The precipitate obtained from the neutralization reaction is ripened, washed and dried, and the dried material is extruded and formed into tablets. The processing agent of the present invention, which is manufactured into a molded product, is filled in a flow type charging tower, and secondly, the metal hydride can be harmed by contacting the reducing exhaust gas containing the metal hydride. As for the metal hydride gases which can be eliminated by the treatment agent of the present invention, there are silane, osmium, phosphine, disilane, diborane, selenium compounds, germanium, dichlorosilane, and the like. Since the treatment agent of the present invention is mainly composed of copper hydroxide or basic copper carbonate, it exhibits a blue-green color, and the adsorption and / or chemical reaction caused by contact with these metal hydride gases will change color, and has The advantages of the processing performance remaining by visually observing the change in color tone were investigated. · # The inventors and others filled the processing agent of the present invention manufactured by a series of operations in a stainless steel flow reactor, and caused a reducing gas containing silane or phosphine containing a metal hydride gas to flow into the reactor. At the same time, the temperature of the treatment agent layer is measured, and the amount of metal hydride gas leakage in the outlet gas is measured by using Brak mnititor (made by Biοnix), and the monitoring is performed, and the destructive performance of the metal hydride-containing gas at room temperature is measured. test. The printed results of the employees ’cooperatives of the Ministry of Economic Affairs and the Smart Finance Bureau have not detected metal hydrides in the outlet gas for a long period of time. Their harmfulness (L / 10 g) is a treatment agent added by a method other than co-sedimentation. Compared with known treatment agents made of the same kind of metal compounds, that is, treatment agents with only effective metal components, or structural stabilizers, it has high performance. Therefore, it is confirmed that the treatment teeth have superior metal hydrogen and are based on oxides. When the same test is carried out for the treatment agent, after the test is started, it is difficult to continue the performance measurement test because the treatment agent layer has a significant increase in the temperature of the abnormal reaction. Although the case of the treatment agent of the present invention can be applied to this paper scale in China National Standard (CNS) Α4 Specification (210 × 29? Mm) "13-'574057
經濟部智慧財產t員工消費合作社印W Α7 Β7 五、發明説明（11 ) 相當程度的發現塡充層之溫度上升，惟確認出引起試驗中 斷的劇烈發熱，以至完成本發明。 圖式之簡單說明 第1圖爲表示鹼性碳酸銅結晶子直徑及矽烷氣體除害 性能之關係圖。 實施發明而採的最佳形態 其次利用實施例再詳細說明本發明之內容。關於本發 明之處理劑，進行金屬氫化物氣體之除害性能測定試驗作 爲性能評估，至於物性評估則進行利用B E T法之表面積 測定及X -射線繞射之金屬化合物的結晶子直徑。在此， 該除害性能測定試驗之測定裝置，測定條件，測定操作方 法，除害性能計算方法係如下所示。 (金屬氫化物氣體之除害性能測定裝置及測定條件） 除害性能測定裝置：常壓流動式反應裝置 反應管尺度：內徑5 Omm，長度1 2 q 〇mm 除害性能測定條件 使用處理劑量：590cc (塡充高度3〇〇min) -^^ 壓力：常壓 反應溫度：常溫 反應氣體組成：S i H4 (或PH3 )1容積％ 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐）~Γ14 .--- (請先閱讀背面之注意事項再填寫本頁)Intellectual Property of the Ministry of Economic Affairs, Employee Cooperative Cooperative Seal W Α7 Β7 V. Description of the Invention (11) The temperature of the filling layer has been increased to a considerable extent, but it has been confirmed that the severe heating that caused the test interruption has led to the completion of the present invention. Brief Description of the Drawings Figure 1 is a graph showing the relationship between the crystal diameter of alkaline copper carbonate and the detoxification performance of silane gas. Best Mode for Carrying Out the Invention Next, the contents of the present invention will be described in detail using examples. Regarding the treatment agent of the present invention, a metal hydride gas detoxification performance measurement test is performed as a performance evaluation, and a physical property evaluation is performed by a surface area measurement using the B E T method and a crystal diameter of a metal compound by X-ray diffraction. Here, the measurement device, measurement conditions, measurement operation method, and calculation method of the detoxification performance measurement test are shown below. (Metal hydride gas detoxification performance measurement device and measurement conditions) Detoxification performance measurement device: atmospheric pressure flow type reaction device Reaction tube dimensions: inner diameter 5 Omm, length 1 2 q 〇mm Determining performance measurement conditions Use treatment dose : 590cc (filling height 300min)-^^ Pressure: atmospheric pressure reaction temperature: room temperature reaction gas composition: S i H4 (or PH3) 1% by volume This paper size applies Chinese National Standard (CNS) A4 specification (210X297 Mm) ~ Γ14 .--- (Please read the notes on the back before filling this page)
574057 A7 B7 經濟部智慧財產—員工消費合作社印製 五、發明説明（12) (Η 2 4容積％ ) Ν 2 餘量 (金屬氫化物氣體之除害性能測定操作方法及除害性能計 算方法） 將處理劑5 9 0 c C塡充於反應管內至塡充高度成 3 0 0 m m並設置於測定裝置，其次使上述組成之金屬氫 化物氣體流通於處理劑塡充層內。氣體開始流通後，進行 處理劑層之溫度測定，同時用black monitor (日本Bionix製 造）測定洩漏至反應管出口氣體中的金屬氫化物氣體，並 予監視，求取其出口濃度達矽烷（SiH4) 5ppm或膦 (ρΗ3) 0·lppm爲止流入的矽烷或膦之積算量， 將該量換算成每lkg處理劑之-量。具體而言，由上述測 定結果依下式計算出金屬氫化物氣體之除害性能。 除害性能（L / k g ) = A X ( B / 1 〇 〇 ) X ( C / E ) 式內，A :測定氣體流量（L /m i η ) Β :金屬氫化物氣體濃度（容積％) C :金屬氫化物氣體之出口濃度達指定濃度爲 止的累積氣體流通時間（m i η ) Ε:處理劑塡充量（kg) 實施例- 1 於2 0 L燒杯內稱取硫酸銅1 · 5 k g，加入純水 1 〇 L，攪拌溶解以製備沈澱母液（A液）。與此另外稱 (請先閱讀背面之注意事項再填寫本頁) 訂 Φ 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -15 - 574057 A7 ______ B7_ _ 五、發明説明（13 ) (請先閱讀背面之注意事項再填寫本頁) 取3號矽酸鈉1 5 %水溶液2 · 1 k g及碳酸鈉0 . 6 2 k g於2 0 L燒杯內，加純水1 〇 L，攪拌，溶解而製備 沈澱劑水溶液（B液）。於經予劇烈攪拌的a液中徐徐滴 下B液，使生成沈澱。將所得的沈澱物熟成後，充分水洗 ，其次過濾後’在空氣中於1 1 〇 t乾燥，而得乾燥粉末 〇 將所得的粉末移入捏練機內，加入適量的純水並充分 混合後，予以擠壓成型。將此成型物在1 1 〇 t乾燥，製 備實施例之含有金屬氫化物之廢氣處理劑。此處理劑之 Cu/S i (原子比），BET表面積及銅化合物之結晶 子直徑係示於表- 1上，於氫氣不存在下的金屬氫化物除 害性能之測定結果示於表- 2。 實施例—2 經濟部智慧財產奇員工消費合作社印製 除實施例- 1之硫酸銅，3號矽酸鈉1 5 %水溶液及 碳酸鈉之使用量各自爲1 . 7kg，1 · 5kg及〇 . 7 k g，藉由於經予劇烈攪拌的B液中徐徐滴下A液，使生 成沈澱外，餘與實施例- 1相同的製備方法製備實施例-2之含有金屬氫化物之廢氣處理劑。此處理劑之C u /574057 A7 B7 Printed by the Intellectual Property of the Ministry of Economic Affairs—Employees' Cooperative Cooperatives 5. Description of the invention (12) (Η24 4% by volume) Ν 2 balance (method for measuring the harm removal performance of metal hydride gas and calculation method for harm removal performance) The treatment agent 590 c C 塡 was filled in the reaction tube to a filling height of 300 mm and installed in a measuring device, and then the metal hydride gas having the above composition was circulated in the treatment agent filling layer. After the gas begins to flow, the temperature of the treatment agent layer is measured. At the same time, the metal hydride gas leaking into the gas at the outlet of the reaction tube is measured with a black monitor (manufactured by Japan Bionix), and monitored to determine the outlet concentration of the silane (SiH4) The total amount of silane or phosphine that has flowed up to 5 ppm or phosphine (ρΗ3) to 0.1 ppm is converted to -amount per 1 kg of the treatment agent. Specifically, from the above measurement results, the detoxifying performance of the metal hydride gas was calculated according to the following formula. Harm removal performance (L / kg) = AX (B / 1 〇) X (C / E) In the formula, A: Measurement gas flow rate (L / mi η) Β: Metal hydride gas concentration (volume%) C: Cumulative gas flow time (mi η) until the outlet concentration of the metal hydride gas reaches the specified concentration. E: Treatment agent charge (kg). Example-1 Weigh 1.5 kg of copper sulfate in a 20 L beaker and add 10 L of pure water was dissolved by stirring to prepare a mother liquor (liquid A). This is also called (please read the precautions on the back before filling this page) Order Φ This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -15-574057 A7 ______ B7_ _ V. Description of the invention (13 ) (Please read the precautions on the back before filling out this page) Take No. 3 sodium silicate 15% aqueous solution 2 · 1 kg and sodium carbonate 0.6 2 kg in a 20 L beaker, add 10 liters of pure water, Stir and dissolve to prepare a precipitant aqueous solution (liquid B). Liquid B was slowly dropped into liquid a which had been vigorously stirred to precipitate. After the obtained precipitate is matured, it is sufficiently washed with water, and then filtered, and dried in air at 110 tons to obtain a dry powder. The obtained powder is transferred into a kneader, and an appropriate amount of pure water is added and mixed thoroughly. Extruded. This molded article was dried at 110 tons to prepare an exhaust gas treating agent containing a metal hydride according to the example. The Cu / S i (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table-1, and the measurement results of the metal hydride removal performance in the absence of hydrogen are shown in Table-2. . Example-2 The printout of the Intellectual Property Owner's Consumer Cooperative of the Ministry of Economic Affairs prints out the copper sulfate of Example-1, the 15% aqueous solution of sodium silicate No. 3 and the use amount of sodium carbonate are 1.7kg, 1.5kg and 〇. 7 kg, because the A liquid was slowly dripped from the B liquid which was vigorously stirred, so that a precipitate was generated, and the same preparation method as in Example -1 was used to prepare an exhaust gas treating agent containing metal hydride of Example-2. C u /
Si (原子比），：BET表面積及銅化合物之結晶子直徑 ^保表 2 5 ~~ ~~" ^ 實施例一 3 除實施例- 1之硫酸銅，3號矽酸鈉1 5 %水溶液及 -16- 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X 297公釐） 574057 Α7 Β7 經濟部智慧財產奇員工消費合作社印製 五、發明説明（14) 碳酸鈉之使用量各自爲1 · 9kg，〇 · 9kg及0 . 9 k g外，餘與實施例- 1相同的製備方法製備實施例- 3 之含有金屬氫化物之廢氣處理劑。此處理劑之C u / S i (原子比），：B E 丁表面積及銅化合物之結晶子直徑係示 於表1 ，於氫氣不存在下的金屬氫化物除害性能之測定結 果示於表一 2。 實施例一 4 除實施例—1之硫酸銅，3號的矽酸鈉1 5 %水溶液 及碳酸鈉之使用量各自爲2 · Okg，〇 . 58kg及 0 . 9 2 k g外餘與實施例一 1相同的製備實施例—4之 含有金屬氫化物之廢氣處理劑。此處理劑之C u / S i ( 原子比），B E T表面積及銅化合物之結晶子直徑係示於 表1 ，於氫氣不存在下的金屬氫化物除害性能之測定結果 不於表一 2。 實施例- 5 除使用碳酸鉀0 . 7 8 k g取代碳酸鈉外，餘以與實 施例- 2相同的製備方法製備實施例- 5之含有金屬氫化 物之廢氣處理劑。此處理劑之C u / S i (原子比）， - 表面子 r 徑Ί 氫氣不存在下的金屬氫化物除害性能之測定結果示於表- (請先閱讀背面之注意事項再填寫本頁) 一裝· .% -1. 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X 297公釐） -17 - 574057 A7 B7 五、發明説明（15) 實施例- 6 (請先閱讀背面之注意事項再填寫本頁) 除使用氫氧化鈉〇 · 4 8 k g取代碳酸鈉外，餘以與 實施例- 2相同的製備方法製備實施例一 6之含有金屬氣 化物之廢氣處理劑。此處理劑之C u / S i (原子比）， B E T表面積及銅化合物之結晶子直徑係示於表一 1 ，於 m氣不存在下的金屬氫化物除害性能之測定結果示於表-2 ° 實施例- 7 除實施例- 2之成型物的乾燥溫度設爲1 8 0 °C以外 ’餘以與實施例- 2相同的製備方法製備實施例- 7之含 有金屬氫化物之廢氣處理劑。此處理劑之C u / S i (原 子比）’ B E T表面積及銅化合物之結晶子直徑係示於表 - 1 ’於氫氣不存在下的金屬氫化物除害性能之測定結果 示於表—2 〇 實施例一 8 經濟部智慧財產奇員工消費合作社印製 除各自使用硝酸銅1 . 6 4 k g，重碳酸鈉 1 . 1 k g取代實施例2之硫酸銅，碳酸鈉外，餘以與實 施例- 2相同的製備方法製備實施例- 8之含有金屬氫化 處理齊卜此處理劑之-C u /乇-i (原 B E T表面積及銅化合物之結晶子直徑係示於表- 1 ，於 氫氣不存在下的金屬氫化物除害性能之測定結果示於表一 本紙張尺度適用中國國家標準（CNS ) A4規格（210X297公釐） -18 - 574057 A7 B7 五、發明説明（16 ) 實施例- 9 (請先閱讀背面之注意事項再填寫本頁) 於2 0 L燒杯內稱取硫酸銅1 · 5 k g ’加入純水 1 ◦ L，攪拌溶解以製備沈澱母液（A液）。與此另外稱 取3號矽酸鈉之1 5 %水溶液2 . 1 k g及碳酸鈉 〇· 6 2 k g於2〇L燒杯內’加純水1 〇 L ’攪拌’溶 解而製備沈澱劑水溶液（B液）。於經予劇烈攪拌的B液 中徐徐滴下A液，使生成沈澱。將所得的沈澱物熟成後’ 充分水洗，其次過濾後，在空氣中於1 1 〇 °C乾燥’而得 乾燥粉末。 將所得的粉末移入捏練機內，加入適量的純水並充分 混合後，予以擠壓成型。將此成型物在1 1 〇 °C乾燥，製 備實施例9之含有金屬氫化物之廢氣處理劑。此處理劑之 C u / S i (原子比），B E T表面積及銅化合物之結晶 子直徑係示於表- 1上，於氫4 %存在下的金屬氫化物除 害性能之測定結果及在除害性能測定的發熱狀況示於表- 經濟部智慧財產喬員工消費合作社印製 實施例—1 ο 除實施例- 9之硫酸銅，3號矽酸鈉1 5 %水溶液及 碳^鈉之使用量各κ g k g外，餘以與實施例9相同的製備方法製備實施例-1 0之含有金屬氫化物之廢氣處理劑。此處理劑之C u/ Si (原子比），BET表面積及銅化合物之結晶子直徑 本紙張尺度適用中國國家標準（CNS ) A4規格（210 X 297公釐） -19- 574057 A7 B7 五、發明説明（17) 係示於表1上，於氫4 %存在下的金屬氫化物除害性能之 測定結果及在除害性能測定的發熱狀況示於表- 3。 實施例一 1 1 除實施例- 9之硫酸銅，3號矽酸鈉1 5 %水溶液及 碳酸鈉之使用量各自爲1 . 9kg ，〇.9kg及0 . 9 k g外，餘以與實施例9相同的製備方法製備實施例-1 1之含有金屬氫化物之廢氣處理劑。此處理劑之C u/ Si (原子比），BET表面積及銅化合物之結晶子直徑 係示於表1 ，於氫4 %存在下的金屬氫化物除害性能之測 定結果及在除害性能測定的發熱狀況示於表- 3。 實施例一 1 2 除實施例- 9之硫酸銅，3號矽酸鈉1 5 %水溶液及 碳酸鈉之使用量各自爲2 . Okg，〇 . 58kg及 〇· 9 2 k g外，餘以與實施例一 9相同的製備方法製備 實施例- 1 2之含有金屬氫化物之廢氣處理劑。此處理劑 之C u / S i (原子比），B E T表面積及銅化合物之結 晶子直徑係示於表1，於氫4 %存在下的金屬氫化物除害 性能之測定結果及在除害性能測定的發熱狀況示於表- 3 實施例—1 3 除使用碳酸鉀0 · 7 8 k g取代實施例—1 〇之碳酸 丨^ 衣-- (請先閲讀背面之注意事項再填寫本頁) 訂 Φ 經濟部智慧財產—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） _ 2〇 - 574057 Α7 Β7 五、發明説明（18 ) 鈉外，餘以與實施例- 1 0相同的製備方法製備實施例-1 3之含有金屬氫化物之廢氣處理劑。此處理劑之C U / Si (原子比），BET表面積及銅化合物之結晶子直徑 係示於表1 ，於氫4 %存在下的金屬氫化物除害性能之測 定結果及在除害性能測定的發熱狀況示於表- 3。 實施例一 1 4 除使用氫氧化鈉0 . 4 8 k g取代實施例—1 〇之碳 酸鈉外，餘以與實施例- 1 2相同的製備方法製備實施例 - 1 4之含有金屬氫化物之廢氣處理劑。此處理劑之C u /Si (原子比），：B E T表面積及銅化合物之結晶子直 徑係示於表1 ，於氫4 %存在下的金屬氫化物除害性能之 測定結果及在除害性能測定的發熱狀況示於表- 3。 實施例一 1 5 除實施例- 1 0的成型物之乾燥溫度設爲1 8 0 °C以 外，餘以與實施例- 1 〇相同的製備方法製備方法製備實 施例- 1 5之含有金屬氫化物之廢氣處理劑。此處理劑之 C u / S i (原子比），B E T表面積及銅化合物之結晶 子直徑係示於表- 1 ，於氫4 %存在下的金屬氫化物除害 能測定的-發激狀況示於表二 實施例一 1 6 ▼裝-- (請先閱讀背面之注意事項再填寫本頁) 、1Τ # 經濟部智慧財產奇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） -21 - 574057 A7 B7 五、發明説明（19 ) 除各自使用硝酸銅1 . 64kg，重碳酸鈉 1 1 k g取代實施例一 1 〇之硫酸銅，碳酸鈉外，餘以 與實施例-1 〇相同的製備方法製備實施例- 1 5之含有 金屬氫化物之廢氣處理劑。此處理劑之C u / S i (原子 比），B E T表面積及銅化合物之結晶子直徑係示於表一 1 ’於氫4 %存在下的金屬氫化物除害性能之測定結果及 在除害性能測定的發熱狀況況示於表- 3。 比較例-1 於2 0 L燒杯內稱取硫酸銅2 · 2 k g，加入純水 1 0 L，攪拌溶解以製備沈澱母液（a液）。與此另外稱 取碳酸鈉1 · Γ 2 k g於2 0 L燒杯內，加入純水1 〇 L ’攪拌，溶解而製備沈澱劑水溶液（B液）。於經予劇烈 攪拌的A液中徐徐滴下B液，使生成沈澱。將所得的沈澱 物熟成後，充分水洗，其次過濾後，在空氣中於1 1 0 °C 乾燥，而得乾燥粉末。 將所得的粉末移入捏練機內，加入適量的純水並充分 混合後，予以擠壓成型。將此成型物在Γ 1 〇 °c乾燥，製 備比較例- 1之含有金屬氫化物之廢氣處理劑。此處理劑 之Cu/Si (原子比），：BET表面積及銅化合物之結 —晶"徑係-氣不#在物除~ 害性能之測定結果示於表- 2。 比較例一 2 1— (请先閱讀背面之注意事項再填寫本頁) 訂Si (atomic ratio): BET surface area and crystal diameter of copper compounds ^ Table 2 5 ~~ ~~ " ^ Example 1 3 Except the copper sulfate of Example-1, No. 3 sodium silicate 15% aqueous solution And -16- This paper size applies Chinese National Standard (CNS) A4 specification (210X 297 mm) 574057 Α7 Β7 Printed by the Intellectual Property Office of the Intellectual Property Department of the Ministry of Economic Affairs Consumption Cooperative of the V. Invention Description (14) The amount of sodium carbonate used is 1 Except for 9 kg, 0.9 kg, and 0.9 kg, the same preparation method as in Example-1 was used to prepare the exhaust gas treating agent containing metal hydride of Example-3. The Cu / Si (atomic ratio), BE surface area and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The measurement results of the metal hydride removal performance in the absence of hydrogen are shown in Table 1. 2. Example 1 4 Except for the copper sulfate of Example -1, the amount of 15% aqueous solution of sodium silicate and sodium carbonate of No. 3 was 2.0 kg, 0.58 kg and 0.92 kg, respectively. 1 The same exhaust gas treating agent as Preparation Example-4 containing metal hydride. The Cu / Si (atomic ratio), B E T surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The measurement results of the metal hydride removal performance in the absence of hydrogen are not shown in Table 1. Example-5 A metal hydride-containing waste gas treating agent of Example-5 was prepared in the same manner as in Example-2 except that potassium carbonate was used to replace sodium carbonate (0.88 g). The C u / S i (atomic ratio) of this treatment agent,-Surface diameter r diameter Ί The measurement results of the metal hydride removal performance in the absence of hydrogen are shown in the table-(Please read the precautions on the back before filling this page ) One pack ·.% -1. This paper size applies to Chinese National Standard (CNS) A4 specification (210X 297 mm) -17-574057 A7 B7 V. Description of the invention (15) Example-6 (Please read the back Note that this page is to be filled in again.) Except using sodium hydroxide 0.48 kg instead of sodium carbonate, the same preparation method as in Example-2 was used to prepare the exhaust gas treating agent containing metal vapor of Example 1-6. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1, and the measurement results of the metal hydride removal performance in the absence of m gas are shown in Table- 2 ° Example-7 Except that the drying temperature of the molded product of Example-2 was set to 180 ° C, the waste gas treatment containing metal hydride of Example-7 was prepared in the same manner as in Example-2 Agent. The Cu / Si (atomic ratio) 'BET surface area and the crystal diameter of the copper compound of this treatment agent are shown in Table-1'The measurement results of the metal hydride removal performance in the absence of hydrogen are shown in Table-2 〇Example 1 Printed by the Consumer Cooperative of Intellectual Property of Intellectual Property of the Ministry of Economic Affairs, except that they use copper nitrate 1.64 kg and sodium bicarbonate 1.1 kg instead of copper sulfate and sodium carbonate of Example 2. -2 The same preparation method as in Preparation Example-8 -C u / 乇 -i containing the metal hydrogenation treatment zibu treatment agent (the original BET surface area and the crystal diameter of the copper compound are shown in Table-1. The measurement results of the metal hydride's detoxifying performance in the presence of the paper are shown in Table 1. The paper size is applicable to the Chinese National Standard (CNS) A4 (210X297 mm) -18-574057 A7 B7 V. Description of the invention (16) Examples-9 (Please read the precautions on the back before filling this page) Weigh out copper sulfate 1 · 5 kg in a 20 L beaker 'Add pure water 1 ◦ L, stir and dissolve to prepare the precipitation mother liquor (Liquid A). Take a 1.5% aqueous solution of No. 3 sodium silicate 2.1 kg Sodium carbonate 0.62 kg was dissolved in a 20 L beaker by adding 10 L of pure water and stirred to prepare a precipitant aqueous solution (Liquid B). Liquid A was slowly dripped into the B liquid which was vigorously stirred to produce a solution. Precipitation. The obtained precipitate is matured and then 'washed thoroughly with water, followed by filtration, and then dried in air at 110 ° C' to obtain a dry powder. The obtained powder is transferred into a kneader, and an appropriate amount of pure water is added and fully After mixing, it is extruded. This molded article is dried at 110 ° C to prepare a metal hydride-containing exhaust gas treating agent of Example 9. C u / S i (atomic ratio) and BET surface area of the treating agent The crystal diameters of copper and copper compounds are shown in Table-1. The measurement results of the metal hydride detoxification performance in the presence of 4% hydrogen and the heating conditions in the detoxification performance measurement are shown in the table. Example printed by a consumer cooperative—1 ο Except for the use of copper sulfate in Example-9, 15% aqueous solution of sodium silicate No. 3 and sodium carbonate κ gkg, the rest of the preparation method is the same as in Example 9 Example-1 Waste of Metal Hydride Treating agent: Cu / Si (atomic ratio), BET surface area and crystal diameter of copper compounds of this treating agent. The paper size is applicable to China National Standard (CNS) A4 specification (210 X 297 mm) -19- 574057 A7 B7 V. Description of the invention (17) is shown in Table 1. The measurement results of the metal hydride detoxification performance in the presence of 4% hydrogen and the heating conditions in the detoxification performance measurement are shown in Table-3. Example 1 11 Except for the copper sulfate of Example-9, the used amounts of 15% aqueous solution of sodium silicate 3 and sodium carbonate were 1.9 kg, 0.9 kg, and 0.9 kg, respectively, with the rest of the examples 9 The same preparation method was used to prepare the exhaust gas treating agent containing metal hydride of Example-1 1. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The results of the measurement of the harmfulness of the metal hydride in the presence of 4% hydrogen and the measurement of the harmfulness The fever status is shown in Table-3. Example 1 12 Except for the copper sulfate of Example-9, the used amounts of 15% aqueous solution of sodium silicate 3 and sodium carbonate were 2.0 kg, 0.58 kg, and 0.92 kg, respectively, and the rest was implemented with Example 1 9 The same preparation method was used to prepare the exhaust gas treating agent containing metal hydride of Example-12. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The results of the measurement of the harmfulness of the metal hydride in the presence of 4% hydrogen and its harmfulness are shown in Table 1. The measured heat generation conditions are shown in Table-3 Example—1 3 Except the use of potassium carbonate 0 · 7 8 kg instead of Example 1-10 carbonic acid 丨 ^ clothing-(Please read the precautions on the back before filling this page) Order Φ Printed by the Intellectual Property of the Ministry of Economic Affairs—Employee Consumer Cooperative Co., Ltd. The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) _ 2〇- 574057 Α7 Β7 V. Description of the invention (18) Except for sodium, the rest is subject to the examples -10 The same preparation method was used to prepare the exhaust gas treating agent containing metal hydride of Example-13. The CU / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The measurement results of the metal hydride removal performance in the presence of 4% hydrogen and Fever conditions are shown in Table-3. Example 1 Except the use of 0.48 kg of sodium hydroxide in place of the sodium carbonate of Example-10, the same preparation method as Example-12 was used to prepare Example-14 containing metal hydride. Exhaust treatment agent. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The measurement results of the metal hydride removal performance in the presence of 4% hydrogen and its performance The measured fever conditions are shown in Table-3. Example 1 15 Except that the drying temperature of the molded product of Example-10 was set to 180 ° C, the same preparation method as in Example-10 was used. Waste gas treatment agent. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table-1, and the deactivation ability of the metal hydride in the presence of 4% hydrogen is measured. In the second embodiment of Table 1 1 6 ▼ Loading-(Please read the precautions on the back before filling in this page), 1T # Printed by the Ministry of Economic Affairs, Intellectual Property, Strange Employees, and Consumer Cooperatives. The paper dimensions are applicable to China National Standard (CNS) Α4 specifications. (210X297 mm) -21-574057 A7 B7 V. Description of the invention (19) Except that copper nitrate 1.64 kg and sodium bicarbonate 11 kg were used instead of copper sulfate and sodium carbonate of Example 10, Example-1 〇 The same preparation method was used to prepare the exhaust gas treating agent containing metal hydride of Example-15. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1 1 'The results of the measurement of the harmfulness of the metal hydride in the presence of 4% hydrogen and The heat generation status of the performance measurement is shown in Table-3. Comparative Example-1 In a 20 L beaker, copper sulfate 2 · 2 k g was weighed, 10 L of pure water was added, and the solution was stirred and dissolved to prepare a precipitation mother liquor (a solution). At the same time, sodium carbonate 1 · Γ 2 kg was weighed into a 20 L beaker, 10 L of pure water was added and stirred, and dissolved to prepare a precipitant aqueous solution (liquid B). Liquid B was slowly dropped into liquid A which had been vigorously stirred to precipitate. The obtained precipitate was aged, washed sufficiently with water, and then filtered, and then dried in air at 110 ° C to obtain a dry powder. The obtained powder was transferred into a kneader, an appropriate amount of pure water was added thereto, and the mixture was thoroughly mixed, followed by extrusion molding. This molded article was dried at Γ 10 ° C to prepare a metal hydride-containing exhaust gas treating agent of Comparative Example-1. The Cu / Si (atomic ratio), BET surface area, and the copper compound junction of this treatment agent-crystals "diameter system-gas does not exist in the body ~ the results of measuring the harmful properties are shown in Table-2. Comparative Example 1 2 1— (Please read the notes on the back before filling this page) Order
經濟部智慧財產焉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（210Χ297公釐） :22 - 574057 Α7 Β7 五、發明説明（2〇 ) 於2 0 L燒杯內稱取3號矽酸鈉1 5 %水溶液1 . 5 k g，加入純水1 〇 L並將5 %硫酸水溶液1 7 0 0 c c 徐徐的滴入已稀釋的水溶液內藉由中和而得沈澱物。藉由 將此充分水洗後，乾燥，粉碎，先行製備矽化合物粉末。 於2 0 L燒杯內稱取硫酸銅1 · 7 k g，加入純水1 〇 L ，攪拌，溶解作爲沈澱母液（A液）。與此另外稱取碳酸 鈉0 · 8 7 k g於2 0 L燒杯內，於加入純水1 〇 L，攪 拌，溶解的溶液內，全量添加事先已先行製備的矽化合物 ，製備沈澱劑水溶液（B液）。於已劇烈攪拌的B液中徐 徐滴下A液，使生成沈澱物。將所得的沈澱物熟成後，充 分水洗，其次過濾後，在空氣中於1 1 〇 °C乾燥，而得乾 燥粉末。 將所得的粉末移入捏練機內，加入適量的純水並充分 混合後，予以擠壓成型。將此成型物在1 1 0 °c乾燥，製 備比較例- 2之含有金屬氫化物之廢氣處理劑。此處理劑 之Cu/Si (原子比），：BET表面積及銅化合物之結 晶子直徑係示於表- 1 ，於氫氣不存在下的金屬氫化物除 害性能之測定結果示於表- 2。 比較例一 3 -除賓-施例--1 之， 碳酸鈉之使用量各自設爲2 _’09kg，0 · 3〇kg及 1 . 0 4 k g外，餘以與實施例—1相同的製備方法製備 比較例- 3之含有金屬氫化物之氣體處理劑。此處理劑之 ▼裝-- (請先閱讀背面之注意事項再填寫本頁) 、1ΤPrinted by the Intellectual Property of the Ministry of Economic Affairs and Employees' Cooperatives. The paper size applies to the Chinese National Standard (CNS) Α4 specification (210 × 297 mm): 22-574057 Α7 Β7 5. Description of the invention (20) Weigh 3 in a 20 L beaker Sodium silicate 15% aqueous solution 1.5 kg, 10L of pure water was added and 5% sulfuric acid aqueous solution 1700 cc was slowly dropped into the diluted aqueous solution and neutralized to obtain a precipitate. This was sufficiently washed with water, dried, and pulverized to prepare a silicon compound powder in advance. 1.7 kg of copper sulfate was weighed into a 20 L beaker, 10 L of pure water was added, stirred, and dissolved as a mother liquor (liquid A). In addition, weigh 0. 8 kg of sodium carbonate in a 20 L beaker, add 10 L of pure water, stir, and dissolve the solution. Add the silicon compound prepared in advance to prepare a precipitant aqueous solution (B liquid). To the B solution which had been vigorously stirred, the A solution was dripped slowly to form a precipitate. The obtained precipitate was aged, washed with water sufficiently, and then filtered, and then dried in air at 110 ° C to obtain a dry powder. The obtained powder was transferred into a kneader, an appropriate amount of pure water was added thereto, and the mixture was thoroughly mixed, followed by extrusion molding. This molded article was dried at 110 ° C to prepare a metal hydride-containing exhaust gas treating agent of Comparative Example-2. The Cu / Si (atomic ratio), BET surface area and copper compound crystal diameter of this treatment agent are shown in Table-1, and the measurement results of the metal hydride removal performance in the absence of hydrogen are shown in Table-2. Comparative Example 1-Except for Bin-Example--1, the amount of sodium carbonate used was set to 2_09kg, 0.30kg, and 1.04kg, respectively, and the rest were the same as in Example-1. Preparation method A metal hydride-containing gas treating agent of Comparative Example-3 was prepared. ▼ Pack of this treatment agent-(Please read the precautions on the back before filling this page), 1T
經濟部智慧財產异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（，10Χ 297公釐） -23- 574057 A7 B7 五、發明説明（21 )Printed by the Intellectual Property of the Ministry of Economic Affairs and the Consumer Cooperative. This paper size applies to Chinese National Standard (CNS) A4 (10 × 297 mm) -23- 574057 A7 B7 V. Description of Invention (21)
Cu/Si (原子比），：BET表面積及銅化合物之結晶 子直徑係不於表1 ，於氫氣不存在下的金屬氫化物除害性 能之測定結果示於表- 2。 比較例一 4 除實施例-1之硫酸銅，3號矽酸鈉1 5 %水溶液及 碳酸鈉之使用量各自設爲0 · 88kg，3 · 80kg及 0 · 2 0 k g外，餘以與實施例—1相同的製備方法製備 比較例- 4之含有金屬氫化物之廢氣處理劑。此處理劑之 C u / S i (原子比），B E T表面積及銅化合物之結晶 子直徑係示於表1 ，於氫氣不存在下的金屬氫化物除害性 能之測定結果示於表- 2。 比較例一 5 於2 0 L燒杯內稱取3號矽酸鈉1 5 %水溶液1 . 5 k g，加入純水1 〇 L並將5 %硫酸水溶液1 7 0 0 c c 徐徐的滴入已稀釋的水溶液內藉由中和而得沈澱物。藉由 將此水洗後，乾燥，先行製備矽化合物粉末。於2 0 L燒 杯內稱取硫酸銅1 . 7 k g，加入純水1 〇 L，攪拌，溶 解作爲沈澱母液（A液）。與此另外稱取碳酸鈉0 . 8 7 劑水溶液（B液）。於已劇烈攪拌的B液中徐徐A液，使 生成沈澱物。將所得的沈澱物熟成後，充分水洗，其次過 濾後，在空氣中於1 1 0 °c乾燥，而得乾燥粉末。 本纸張尺度適用中國國家標準(CNS ) A4規格（210X297公釐) -24 - ' ； 批衣— (請先閱讀背面之注意事項再填寫本頁) 訂 經濟部智慧財產焉員工消費合作社印製 574057 經濟部智慧財產局員工消費合作社印製 A7 B7 五、發明説明（22) 將所得的粉末移入捏練機內，加入適量的純水並充分 混合後，予以擠壓成型。將此成形物在1 1 〇 °c乾燥，製 備比較例- 2之含有金屬氫化物之廢氣處理劑。此處理劑 之Cu/Si (原子比），BET表面積及銅化合物之結 晶子直徑係示於表- 1 ，於氣氣4 %存在下的金屬氫化物 除害性能之測定結果及在除害性能測定之發熱狀況示於表 —3 〇 比較例一 6 除以實施例- 9之硫酸銅，3號的矽酸鈉1 5 %水溶 液及碳酸鈉使用量各自設爲2 · 09kg，0 · 30kg ，1 . 0 4 k g外，餘以與實施例一 9相同的製備方法製 備比較例- 6之含有金屬氫化物之廢氣處理劑。此處理劑 之Cu/Si (原子比），：BET表面積及銅化合物之結 晶子直徑係示於表1 ，於氫氣4 %存在下的金屬氫化物除 害性能之測定結果及在除害性能測定之發熱狀況示於表-3。 比較例一 7 除以實施例- 9之硫酸銅’ 3號政酸納1 5 %水溶液 及碳酸胁每用量各0 · 〇.2 0 k g外，餘以與實施例- 9相同的製備方法製備 比較例- 7之含有金屬氫化物之廢氣處理劑。此處理劑之 Cu/S i (原子比），BET表面積及銅化合物之結晶 本紙張尺度適用中國國家標準（CNS ) A4規格（ 210 X297公釐) -25- (請先閲讀背面之注意事項再填寫本頁)Cu / Si (atomic ratio), BET surface area and crystal diameter of copper compounds are not shown in Table 1. The measurement results of metal hydride removal performance in the absence of hydrogen are shown in Table-2. Comparative Example 1 Except for the copper sulfate of Example-1, the amount of 15% aqueous solution of sodium silicate 3 and the amount of sodium carbonate were set to 0. 88 kg, 3. 80 kg, and 0. 20 kg, respectively. Example-1 The same preparation method was used to prepare the exhaust gas treating agent containing metal hydride of Comparative Example-4. The Cu / Si (atomic ratio), B E T surface area, and crystal diameter of copper compounds of this treatment agent are shown in Table 1. The results of the measurement of the metal hydride removal performance in the absence of hydrogen are shown in Table-2. Comparative Example 5 In a 20 L beaker, weighed 1.5 kg of a 15% aqueous solution of No. 3 sodium silicate, added 10 L of pure water, and slowly dripped 1 70 cc of a 5% sulfuric acid solution into the diluted A precipitate is obtained by neutralization in the aqueous solution. The silicon compound powder was prepared by washing this water and drying it. In a 20 L beaker, weigh 1.7 kg of copper sulfate, add 10 L of pure water, stir, and dissolve it as the precipitation mother liquor (Liquid A). In addition, a sodium carbonate 0.8 aqueous solution (B solution) was weighed separately. The solution A was slowly stirred in the solution B which had been vigorously stirred to form a precipitate. After the obtained precipitate was aged, it was sufficiently washed with water, followed by filtration, and then dried in air at 110 ° C to obtain a dry powder. This paper size applies to China National Standard (CNS) A4 specification (210X297 mm) -24-'; Approval — (Please read the precautions on the back before filling this page) Order printed by the Ministry of Economic Affairs Intellectual Property 焉 Employee Consumer Cooperative 574057 Printed by A7 B7, Consumer Cooperatives, Bureau of Intellectual Property, Ministry of Economic Affairs. 5. Description of the invention (22) Move the obtained powder into the kneading machine, add an appropriate amount of pure water and mix thoroughly, and then extrude. This formed article was dried at 110 ° C to prepare a metal hydride-containing exhaust gas treating agent of Comparative Example-2. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table-1. The measured heat generation conditions are shown in Table-3. Comparative Example 6 Divided by the copper sulfate of Example-9, the 15% aqueous solution of sodium silicate No. 3 and the use amount of sodium carbonate were set to 2.09kg and 0.30kg, respectively. Except for 1.0 kg, the same preparation method as in Example 1-9 was used to prepare a metal hydride-containing exhaust gas treating agent of Comparative Example-6. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The measurement results of the metal hydride detoxification performance in the presence of 4% hydrogen and the determination of the detoxification performance The fever conditions are shown in Table-3. Comparative Example 7 Except for the use of copper sulfate of No. 3 in Example-9, a 15% aqueous solution of sodium sulphate and a carbonic acid content of 0. 0.20 kg each, and the rest were prepared in the same manner as in Example-9. Comparative Example-7 A metal hydride-containing exhaust gas treating agent. Cu / S i (atomic ratio), BET surface area and crystallization of copper compounds of this treatment agent The paper size is applicable to Chinese National Standard (CNS) A4 specification (210 X297 mm) -25- (Please read the precautions on the back first (Fill in this page)
574057 A7 B7 經濟部智慧財產肯員工消費合作社印製 五、發明説明（23 ) 子直徑係示於表1 ，於氫氣4 %存在下的金屬氫化物除害 性能之測定結果及在除害性能測定之發熱狀況示於表一 3 〇 比較例一 8 除在3 5 0 °C進行成型物之燒成以取代實施例一 9之 成型物之乾燥，製成氧化物外，餘以與實施例一 9相同的 製備方法製備比較例- 9之含有金屬氫化物之廢氣處理劑 。此處理劑之Cu/Si (原子比），BET表面積及銅 化合物之結晶子直徑係示於表一 1 ，於氫氣4 %存在下的 金屬氫化物除害性能之測定結果及在除害性能測定之發熱 狀況示於表一 3。 比較例一 9 除在3 5 0 °C進行成型物之燒成以取代實施例一 1 1 之成型物之乾燥，製成氧化物外，餘以與實施例一 9相同 的製備方法製備比較例- 9之含有金屬氫化物之廢氣處理 劑。此處理劑之C u / S i (原子比），：B E T表面積及 銅化合物之結晶子直徑係示於表- 1 ，於氫氣4 %存在下 的金屬氫化物除害性能之測定結果及在除害性能測定之發 熱狀況示於表- 3 ~~^ ~~---— (請先閲讀背面之注意事項再填寫本頁)574057 A7 B7 Printed by the Intellectual Property of the Ministry of Economic Affairs, Kennedy Consumer Cooperative, V. Description of the invention (23) The diameter of the sub-system is shown in Table 1, and the measurement results of the metal hydride detoxification performance in the presence of 4% hydrogen and the detoxification performance measurement The heat generation conditions are shown in Table 1 30. Comparative Example 8 Except that the molding was fired at 350 ° C to replace the drying of the molding of Example 9 to make oxides, the rest was the same as in Example 1. 9 The same preparation method was used to prepare a metal hydride-containing exhaust gas treating agent of Comparative Example-9. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table 1. The measurement results of the metal hydride detoxification performance in the presence of 4% hydrogen and the determination of the detoxification performance The fever situation is shown in Table 1. Comparative Example 1 A comparative example was prepared by the same preparation method as in Example 1 except that the molding was fired at 350 ° C to replace the drying of the molded object in Example 1 1 to make an oxide. -9 exhaust gas treatment agent containing metal hydride. The Cu / Si (atomic ratio), BET surface area, and crystal diameter of the copper compound of this treatment agent are shown in Table-1. The measurement results of the metal hydride detoxification performance in the presence of 4% hydrogen and The heating status of the harmful performance measurement is shown in the table-3 ~~ ^ ~~ ---- (Please read the precautions on the back before filling this page)
裝_Outfit_
、1T % 本紙張尺度適用中國國家標準（CNS ) Α4規格（210X297公釐） -26- 574057 A7 B7 五、發明説明（24 ) 經濟部智慧財產*員工消費合作社印製 〔表1〕含有金屬氫化物之氣體處理劑之成分組成比及物 性測定結果 Cu/Si BET表面積 銅化合物之結 (原子比） (m2/g) 晶子直徑（nm) 實施例-1 1.54/1 320 4 實施例-2 2.11/1 250 8 實施例-3 4.56/1 180 15 實施例-4 7.43/1 120 40 實施例-5 2.44/1 230 10 實施例-6 2.44/1 220 12 實施例-7 2.44/1 230 9 實施例-8 2.44/1 260 6 實施例-9 1.54/1 320 4 實施例-1 0 2.44/1 250 8 實施例-11 4.56/1 180 15 實施例-12 7.43/1 120 40 實施例-1 3 2.44/1 230 10 實施例-14 2.44/1 220 12 實施例-1 5 2.44/1 230 9 實施例-16 2.44/1 260 6 比較例-1 僅含有Cu 50 100 比較例-2 2.44/1 80 74 比較例-3 15.0/1 90 69 比較例-4 0.50/1 420 非晶質 1— (請先閱讀背面之注意事項再填寫本頁)、 1T% This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) -26- 574057 A7 B7 V. Description of invention (24) Printed by Intellectual Property of the Ministry of Economic Affairs * Employee Consumer Cooperative [Table 1] Contains metal hydrogenation Composition ratio and physical property measurement result of gas processing agent of the material Cu / Si BET surface area Cu compound (atomic ratio) (m2 / g) Crystal diameter (nm) Example-1 1.54 / 1 320 4 Example-2 2.11 / 1 250 8 Example-3 4.56 / 1 180 15 Example-4 7.43 / 1 120 40 Example-5 2.44 / 1 230 10 Example-6 2.44 / 1 220 12 Example-7 2.44 / 1 230 9 Implementation Example-8 2.44 / 1 260 6 Example-9 1.54 / 1 320 4 Example-1 0 2.44 / 1 250 8 Example-11 4.56 / 1 180 15 Example-12 7.43 / 1 120 40 Example-1 3 2.44 / 1 230 10 Example-14 2.44 / 1 220 12 Example-1 5 2.44 / 1 230 9 Example-16 2.44 / 1 260 6 Comparative Example-1 Only Cu 50 100 Comparative Example-2 2.44 / 1 80 74 Comparative Example-3 15.0 / 1 90 69 Comparative Example-4 0.50 / 1 420 Amorphous 1— (Please read the precautions on the back before filling this page)
、1T, 1T
本紙張尺度適用中國國家標準（CNS ) A4規格（ 210X297公釐） -27 - 574057 A7 B7 五、發明説明（25 ) 比 較 例-5 2.44/1 80 74 比 較 例-6 15.0/1 90 69 比 較 例-7 0.50/1 420 非晶質 比 較 例-8 1.54/1 290 7 比 較 例-9 4.56/1 150 23 經濟部智慧財產—員工消費合作社印製 〔表2〕處理劑之金屬氫化物氣體除害性能測定結果（不 含有H2之含有金屬氫化物之氣體） SiH4(L/kg) PH3(L/kg) 實施例-1 38 87 實施例-2 45 105 實施例-3 40 102 實施例-4 35 85 實施例-5 43 100 實施例-6 40 98 實施例-7 36 80 實施例-8 44 107 比較例-1 20 41 比較例-2 25 47 比較例-3 18 35 比較例-4 17 30 (請先閱讀背面之注意事項再填寫本頁)This paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) -27-574057 A7 B7 V. Description of the invention (25) Comparative Example-5 2.44 / 1 80 74 Comparative Example-6 15.0 / 1 90 69 Comparative Example -7 0.50 / 1 420 Amorphous Comparative Example-8 1.54 / 1 290 7 Comparative Example-9 4.56 / 1 150 23 Printed by the Intellectual Property of the Ministry of Economic Affairs-Employed Consumer Cooperatives [Table 2] Removal of metal hydride gas from treatment agents Performance measurement results (H2-free metal hydride-containing gas) SiH4 (L / kg) PH3 (L / kg) Example-1 38 87 Example-2 45 105 Example-3 40 102 Example-4 35 85 Example-5 43 100 Example-6 40 98 Example-7 36 80 Example-8 44 107 Comparative Example-1 20 41 Comparative Example-2 25 47 Comparative Example-3 18 35 Comparative Example-4 17 30 ( (Please read the notes on the back before filling out this page)
訂 Φ 本纸張尺度適用中國國家標準（CNS ) A4規格（2!0X297公釐） -28 - 574057 A7 B7 五、發明説明（26 ) 經濟部智慧財產局員工消費合作社印製 〔表3〕處理劑之含有金屬氫化物之氣體除害性能測定結 果（含有Η 2 4 %之含有金屬氫化物之氣體） SiH^ (L/kg) PH3 (L/kg) 在性能測定之發熱狀況 (上昇溫度） SiHU PH3 實施例-9 40 90 50 〜60〇C 35 〜45〇C 實施例-10 44 108 50 〜60°C 35 〜45〇C 實施例-11 41 105 50 〜60〇C 35 〜45t： 實施例-1 2 37 87 50 〜60。。 35 〜45〇C 實施例-1 3 45 104 50 〜60。。 35 〜45〇C 實施例-14 41 101 50 〜6(TC 35 〜45°C 實施例-1 5 38 83 50 〜60〇C 35 〜45〇C 實施例-16 46 110 50 〜60°C 35 〜45〇C 比較例-5 25 47 45 〜55°C 30 〜40〇C 比較例-6 19 26 40 〜50〇C 30 〜35〇C 比較例-7 18 32 40 〜50〇C 30 〜35〇C 比較例-8 由於不正常反 由於不正常反 比較例-9 應而中止測定 應而中止測定 產業上之可利用性 氣氧化銅或鹼性碳酸銅與矽化合物之混合物或各該銅 合物及砂化合物之一部分由於係痕成複合體之混合扬， 故可得金屬氫化物氣體之除害性能較高的低發熱性之含有 金屬氫化物廢氣處理劑，於有金屬成分之因氫引起的還原 之可能性的廢氣處理，係有效的。 本紙張尺度適用中國國家標準（CNS ) A4規格（ 210X297公釐） I 29 - " (請先閱讀背面之注意事項再填寫本頁)Order Φ This paper size applies Chinese National Standard (CNS) A4 specification (2! 0X297 mm) -28-574057 A7 B7 V. Description of the invention (26) Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs [Table 3] Measurement results of the detoxification performance of the metal hydride-containing gas (containing Η 24% of the metal hydride-containing gas) SiH ^ (L / kg) PH3 (L / kg) Heating condition (rise temperature) in performance measurement SiHU PH3 Example-9 40 90 50 to 60 ° C 35 to 45 ° C Example-10 44 108 50 to 60 ° C 35 to 45 ° C Example-11 41 105 50 to 60 ° C 35 to 45t: Implementation Example-1 2 37 87 50 to 60. . 35 to 45 ° C Example-1 3 45 104 50 to 60. . 35 ~ 45 ° C Example-14 41 101 50 ~ 6 (TC 35 ~ 45 ° C Example-1 5 38 83 50 ~ 60 ° C 35 ~ 45 ° C Example-16 46 110 50 ~ 60 ° C 35 ~ 45 ° C Comparative Example-5 25 47 45 to 55 ° C 30 to 40 ° C Comparative Example-6 19 26 40 to 50 ° C 30 to 35 ° C Comparative Example-7 18 32 40 to 50 ° C 30 to 35 〇C Comparative Example-8 Abnormal due to abnormal response Comparative Example-9 Due to abnormal response, the measurement should be suspended Due to industrial availability Gas copper oxide or a mixture of basic copper carbonate and a silicon compound or each of the copper compounds Some of the compounds and sand compounds are mixed with the traces to form a complex, so a metal hydride gas-containing low-heat-generating waste gas treatment agent with high destructive performance can be obtained. Exhaust gas treatment with the possibility of reduction is effective. This paper size applies Chinese National Standard (CNS) A4 specification (210X297 mm) I 29-" (Please read the precautions on the back before filling this page)
衣· 、-ιτ %Clothing ·, -ιτ%
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW90116046A TW574057B (en) | 2001-06-29 | 2001-06-29 | Treating agent for exhaust gas containing metal hydride, process for producing the same, and method of treating exhaust gas containing metal hydride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| TW90116046A TW574057B (en) | 2001-06-29 | 2001-06-29 | Treating agent for exhaust gas containing metal hydride, process for producing the same, and method of treating exhaust gas containing metal hydride |
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