TW419531B - Removal of fluoride-containing scales using aluminum salt solution - Google Patents
Removal of fluoride-containing scales using aluminum salt solution Download PDFInfo
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A7 B7 玉 經濟部中央標绛局員工消費合作社印製 更特别而言,係自 4 195 3 發明説明( 發明背景 1. 發明領域 本發明係有關自金屬表面移除垢, 金屬表面移除含氯化物之垢。 2. 習知技術之描述 當煤或其它含灰之有機材料於高麗、高溫之部份氧化 棘冷氣化线巾氣化時’紐材料騎變絲似、細微 礦潰與水溶性灰爐組份間之分隔。水被用於系統中以使供 料煤呈敷料’驟冷熱合成氣體,亦稱為“合成氣,,且驟冷 熱礦渣副產物$水亦被用於使顆粒物料自合成氣洗滌出, 且於輸送中促進礦渣副產物離開氣化器β 氟化辦及氟化鎮垢,其形成於蒸發器管線上,通常係 以無機酸(諸如,硫酸、氮氣酸或确’酸)化學移除之。當 咸酸被用於鋼垢移除時,通常會沈澱Cas〇4。於酸清理氟 化物垢時’腐姓性之氫氟酸形成於清淅溶液内.,且含有金 屬及金屬合金(諸如,鈦、鎳及不鏽鋼),其會易於由氫 氟酸嚴重腐蝕。溶液中氟化物離子(F·)之存在與形成於此 等金屬上之保護性氧化物相干擾,且使鈦、鐵及鎳離子溶 於酸性溶液。因此,於處理裝置中僅使用酸來化學清理氟 化物垢係不實際。亦需注意鈣垢可藉由使用乙二胺四乙酸 化學移除之。 垢亦可藉由機械裝置移除之,諸如,刮削或以鐵鎚撞 擊或以水衝擊。但是,化學清理較佳且較常用,因為垢可 於水衝擊喷嘴無法到達處被溶解移除之。因此’期望自以 本纸浪尺度適用中國國家榡準(CNS ) A4規格(210X 297公釐) (請先閲讀背面之注意事項再填寫本頁) 订 4 經濟部中央標隼局員工消費合作社印製 4195 31 A7 B7 ~ " 五·、發明説明(2 ) 鈦或不鏽鋼構成之裝置化學溶解氟化物垢。鈦及不鏽鋼通 常被用於廢水處理工業,特別是廢水蒸發器結構。 文獻亦強調於不鏽鋼、鎳合金及鈦合金製成之處理裝 置之氫氟酸腐蝕之問題。Koch, G.H.,“非氯化物之鹵化物 之局部腐蝕”,環境並用1993年6月,揭示鐵或鋁離子 可抑制腐钱。 燃料氣體脫硫處理滌氣器内水溶液作用及其腐蝕性亦 已被研討。此等溶液含氯化物、氟化物及硫化物(於低pH 值),例如’於pH=l時為4800 mg/kg氟化物。添加燃料 灰燼礦物質C其含有明顯量之矽、鐵及鋁)可抑制其它侵 略性含氟化物溶液中之鈦腐蝕。亦發現若10,000 mg鋁/kg (以硫酸鋁添加)被添加至含10,000 11^/4氣化物及 1,000 mg/kg氟化物之腐蝕性酸溶液,溶液不再對鈦具腐 银性。 發明之綜述 含氟化物垢可藉由使金屬表面與無機酸之水溶性鹽溶 液(包括其水和物)接觸而自金屬表面(諸如,鈦、敛合 金、錄合金及不鏽鋼)移除。鹽類之陽離子部份可為链、 鐵及其^合。鹽類之陰離子部份可為氯化物、硝酸鹽、硫 酸鹽及其混合物》接觸係發生於無添加酸(諸如,氫氣酸 、硝酸或硫酸)。具溶解之氯化物垢之水性鹽溶液之存在 不會促進或增加會發生於缺乏水性鹽溶液或任何酸清潔劑 之金屬腐蝕之正常速率《 較佳實施例之描述 本紙法尺度適用t國國家標準(CN’S ) A4規格(210X297公逢) (請先閎讀背面之注意事項再填寫本頁) -訂A7 B7 Printed by the Consumers' Cooperative of the Central Bureau of Standards, Jade Ministry of Economy More specifically, it is from 4 195 3 Invention Description (BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to removing scale from metal surfaces and removing chlorine from metal surfaces 2. Description of the conventional technology. When coal or other ash-containing organic materials are gasified in Korean and high-temperature partial oxidized cold gasification line towels, the button materials become silky, fine ore collapse, and water-soluble. Separation between the components of the ash furnace. Water is used in the system to make the feed coal as a dressing 'quenching hot synthetic gas, also known as "syngas," and quenching hot slag by-product $ water is also used to make granular materials It is washed out from synthesis gas and promotes the slag by-products to leave the gasifier β fluorination office and fluorinated scale during transportation. It is formed on the evaporator pipeline and is usually made of inorganic acids such as sulfuric acid, nitrogen acid or acetic acid. 'Acid) is chemically removed. When salty acid is used for the removal of steel scale, Cas0 4 is usually precipitated. When the acid is used to clean up the fluoride scale,' corrosive hydrofluoric acid is formed in the clear solution., And contains metals and metal alloys (such as titanium Nickel and stainless steel), which can be easily corroded by hydrofluoric acid. The presence of fluoride ions (F ·) in the solution interferes with the protective oxides formed on these metals and dissolves titanium, iron and nickel ions. In acidic solution. Therefore, it is not practical to use only acid to chemically clean up fluoride scale in the treatment device. It should also be noted that calcium scale can be chemically removed by using ethylenediaminetetraacetic acid. Scale can also be removed by mechanical devices In addition, such as scraping or impacting with a hammer or impacting with water. However, chemical cleaning is better and more commonly used because dirt can be removed by dissolution where water impact nozzles cannot reach. Therefore, 'I hope that the paper waves Standards are applicable to China National Standards (CNS) A4 specifications (210X 297 mm) (Please read the notes on the back before filling out this page) Order 4 Printed by the Central Consumers Bureau of the Ministry of Economic Affairs Consumer Cooperatives 4195 31 A7 B7 ~ " V. Description of the invention (2) The device made of titanium or stainless steel chemically dissolves fluoride scale. Titanium and stainless steel are usually used in wastewater treatment industry, especially the structure of wastewater evaporator. The literature also emphasizes on stainless steel and nickel alloy. Problems of Hydrofluoric Acid Corrosion of Processing Equipment Made of Gold and Titanium Alloys. Koch, GH, "Localized Corrosion of Non-Chloride Halides", Environmental Use June 1993, revealed that iron or aluminum ions can inhibit rotten money. The role of aqueous solutions in scrubbers of fuel gas desulfurization scrubbers and their corrosivity have also been studied. These solutions contain chlorides, fluorides and sulfides (at low pH), such as' 4800 mg / at pH = 1 kg of fluoride. Addition of fuel ash mineral C which contains significant amounts of silicon, iron and aluminum) can inhibit the corrosion of titanium in other aggressive fluoride-containing solutions. It was also found that if 10,000 mg aluminum / kg (added with aluminum sulfate) was used Add to a corrosive acid solution containing 10,000 11 ^ / 4 gas and 1,000 mg / kg fluoride. The solution is no longer corrosive to titanium. Summary of the Invention Fluoride-containing scales can be removed from metal surfaces (such as titanium, alloys, alloys, and stainless steel) by contacting the metal surface with a water-soluble salt solution of an inorganic acid (including its water and matter). The cationic portion of the salt may be a chain, iron, or a combination thereof. The anionic part of salts can be chlorides, nitrates, sulfates, and mixtures thereof. Contact occurs in the absence of added acids (such as hydrogen acid, nitric acid, or sulfuric acid). The presence of an aqueous salt solution with dissolved chloride scale does not promote or increase the normal rate of metal corrosion that would occur in the absence of an aqueous salt solution or any acid cleaner. "Description of the preferred embodiment" (CN'S) A4 specification (210X297) (please read the precautions on the back before filling this page)-Order
-T 4195 31 A7 B7_______ 五、發明説明(3 ) 為保存水’氣化系統操作單元尋求再循環處理水,通 常係於純化處理後,諸如,移除固體沈降器内細微顆粒礦 渣或“礦渣微粒”。因氣化反應藉由於合成氣體内產生氫 來消耗水,通常無需自系統移除水來避免沈積。然而,一 部份之處理廢水(亦稱為水性流出物、灰水或排放水)通 常以清洗廢水流自系統移除,以避免過量生成腐蝕性鹽類 ,特別是氯化物鹽。 如第1表所示,其依循高氣化物Eastern US煤之氣化 資料,自氣化系統流出之排放廢水之組成相當複雜。對於 具相對高含量氣化物之原料,主要廢水組份為氯化銨。 第1表 高氣化物美東煤之灰燼含量 氣化器供料煤 (流速=71,95〇公升/小時) 排放水 (流速=33,208公升/小時) 水中煤料 之百分率 灰燼種類 濃度 質流 (克/小時) 濃度 質流 (克/小時) 氨N 1.4% 1007300 1500 mg/L 49812 4.95 納 590 mg/g 42450.5 32mg/L 1063 2.50 1200.mg/g 86340 12 mg/L 398 0.46 鋁 10000 mg/g 719500 2.3 mg/L 76 0.01 鈣 2600 mg/g 187070 20 mg/L 664 0.36 鎂 700 mg/g 50365 4.3 mg/L 143 0.28 硼 54 mg/g 3885.3 37 mg/L 1229 31.62 氣化物 0.2% 86340 2600 mg/L 86341 ^ 100.0 氟化物 0.019% 13670.5 63 mg/L 2092 15.30 甲酸鹽 — 0 770 mg/L 25570 — 矽 19000 mg/g 1367050 60 mg/L 1992 0.15 灰爐中發現之某些材料為部份水溶性,即,一部份材 料保留於固體礦渣或灰燼微粒,而一部份溶於水中。例如 ’鋼及鉀化合物以其離子溶於水中,而以固體材料保留於 本紙張尺度適用中國國家標準(〇JS ) A4规格(210 X 297公釐) ,6 - (請先閲讀背面之注意事項再填寫本頁) 0Γβ------訂------一'· 經濟部中央標準局—工消費合作社印製 4 195 31 經濟部中央標準局員工消费合作社印製 A7 B7 五、發明説明(4 ) 固體中。硼化合物以硼酸及硼酸鹽離子溶於水中,而以氧 化蝴碌物質留於固體内。鋁、矽、鈣及鎂化合物主要係不 可溶,而氟化物亦係主要為不可溶。 因由氣化系統排出之廢水含有鹽類及其它潛在之環境 有害'纟且份’因此需於水被排放前處理之。各種污染物之廢 水處理會有點複雜及昂貴,因此,期望有其它用以處理廢 水之經濟方法。 於某些條件下蒸餾廢水或海水為一種自廢水回收相對 砘艮之有效且經濟之方法。適當之蒸顧氣化廢水之方法包 括落膜蒸發及強迫性循環蒸發。本發明係提供移除形成於 蒸發器及其它任何裝置之金屬表面上之氟化物垢之方式。 於落膜蒸發中,主要系統熱交換器為垂直β欲被蒸發 之海水係被引至熱交換器管之頂部且自底部回收。海水係 由位於熱交換器管低部之海水槽泵取入管線頂部。海水以 内管壁上之膜狀物經由管線向下落,接收熱,如此,其内 所含之水蒸發而於海水下降時形成蒸氣。海水與蒸氣之藏 合物流出熱交換器管之底部且進入海水槽,其間水蒸氣與 濃縮液體海水分離之。蒸氣自海水槽之底部流出,且殘留 之濃縮液體海水於海水槽内收集,其間藉自录循環至熱交 換器管之頂部。然後,蒸氣被冷凝形成水蒸顧液,其可被 回流至氣化系統。供料水(諸如,自氣化系統流出之廢水 )連續添加至海槽’且—部份濃縮海水被連續回收以 祚為結晶用且回收其内所含之濃縮鹽。 於強力循環蒸發中,主要系統^交換器為水平,其具 (請先閱讀背面之注意事項再填寫本育) — I1T------.. 張 紙 本 適 一格 規 f釐 公 7 4195 31 經濟部中央標準局員工消費合作社印製 A7 B7 發明説明(5 ) 有經管線泵取之液體海水及於交換器之殼側引入以加熱海 水之蒸氣。海水於流經管線時並未沸騰,因為其内之足夠 壓力可避免浠騰。然後’由交換器管流出之熱海水向上轉 移至位於熱交換器上方上海水槽。於海水向上流動時,壓 力下降且熱海水沸騰而形成濃縮海水與水蒸氣之二相混合 物。當二相混合物進入海水槽時,水蒸氣與海水分離,且 離開海水至冷凝器’其間水蒸氣被冷凝形成蒸餾水。海水 藉由循環泵被回收至蒸發器,其一部份以海水下流移除以 作為進一步之鹽結晶及回收。再者當以落膜蒸發器時,供 料水被添加至海水槽或至海水猶環線。 雖然落膜及強力循環蒸發器為一般用於水蒸德應用, 其使用性係依據形成之速率及於蒸發器熱交換器表面之累 積而定β自蒸發器熱交換器及橹表面移除垢係非常重要, 因為於裝置表面上之垢形成係作為絕緣物且需週期性移除 ,以便有效地操作蒸發器單元。 第2表所示之垢之組成物係由氣化灰水之蒸發作用形 成’其中落膜及強力循環蒸發器係系列使用之。主要之垢 成份為氧化矽(Si02)、氟化鈣(CaF2)及氟化鎂(MgF2)。 (請先閲讀背面之注意事項再填寫本頁)-T 4195 31 A7 B7_______ V. Description of the invention (3) To recycle the treated water for the gasification system operation unit, usually after purification treatment, such as removing fine-grained slag or "slag particles" in the solid settler ". Because the gasification reaction consumes water by generating hydrogen in the synthesis gas, it is generally not necessary to remove water from the system to avoid deposition. However, a portion of the treated wastewater (also known as aqueous effluent, grey water, or effluent) is usually removed from the system by a cleaning wastewater stream to avoid excessive formation of corrosive salts, especially chloride salts. As shown in Table 1, according to the gasification data of the high gaseous Eastern US coal, the composition of the discharged wastewater discharged from the gasification system is quite complicated. For raw materials with relatively high gaseous content, the main wastewater component is ammonium chloride. Table 1 Ash content of high gasification Meidong coal gasifier coal feed (flow rate = 71,95 liters / hour) discharged water (flow rate = 33,208 liters / hour) percentage of coal in water ash species concentration mass flow ( G / h) concentration mass flow (g / h) ammonia N 1.4% 1007300 1500 mg / L 49812 4.95 nano 590 mg / g 42450.5 32mg / L 1063 2.50 1200.mg/g 86340 12 mg / L 398 0.46 aluminum 10000 mg / g 719500 2.3 mg / L 76 0.01 calcium 2600 mg / g 187070 20 mg / L 664 0.36 magnesium 700 mg / g 50365 4.3 mg / L 143 0.28 boron 54 mg / g 3885.3 37 mg / L 1229 31.62 gas 0.2% 86340 2600 mg / L 86341 ^ 100.0 Fluoride 0.019% 13670.5 63 mg / L 2092 15.30 Formate — 0 770 mg / L 25570 — Silicon 19000 mg / g 1367050 60 mg / L 1992 0.15 Some materials found in the ash furnace are internal Part water-soluble, that is, part of the material remains in solid slag or ash particles, and part is dissolved in water. For example, 'steel and potassium compounds dissolve in water with their ions, and solid materials are kept at the standard of this paper. Chinese national standard (〇JS) A4 specification (210 X 297 mm), 6-(Please read the precautions on the back first (Fill in this page again.) 0Γβ ------ Order ------ 一 '· Printed by the Central Standards Bureau of the Ministry of Economic Affairs-Consumer Cooperatives 4 195 31 Printed by the Central Consumers Cooperative of the Ministry of Economic Affairs A7 B7 Description of the invention (4) in solid. The boron compound is dissolved in water with boric acid and borate ions, and remains in the solid as an oxygenated substance. Aluminum, silicon, calcium and magnesium compounds are mainly insoluble, while fluorides are mainly insoluble. The waste water discharged from the gasification system contains salts and other potentially harmful environmental factors, so it needs to be treated before the water is discharged. Wastewater treatment of various pollutants can be a bit complicated and expensive, so other economic methods for treating waste water are desired. Distilling wastewater or seawater under certain conditions is a relatively efficient and economical way to recover from wastewater. Appropriate methods for vaporizing wastewater include falling film evaporation and forced circulation evaporation. The present invention provides a way to remove fluoride scale formed on metal surfaces of evaporators and any other devices. In falling film evaporation, the main system heat exchanger is vertical β. The seawater to be evaporated is led to the top of the heat exchanger tube and recovered from the bottom. Seawater is pumped into the top of the pipeline by a seawater tank pump located at the lower part of the heat exchanger tube. The membrane on the inner tube wall drops down through the pipeline to receive heat. In this way, the water contained in it evaporates to form steam when the seawater drops. The mixture of seawater and steam flows out of the bottom of the heat exchanger tube and enters the seawater tank, during which the water vapor is separated from the concentrated liquid seawater. Vapor flows from the bottom of the seawater tank, and the remaining concentrated liquid seawater is collected in the seawater tank, during which it is self-circulated to the top of the heat exchanger tube. The vapor is then condensed to form a water distillate, which can be returned to the gasification system. Feed water (such as waste water flowing from the gasification system) is continuously added to the trough 'and-part of the concentrated seawater is continuously recovered for the hydration for crystallization and the concentrated salt contained therein is recovered. In the strong circulation evaporation, the main system ^ exchanger is horizontal, and it has (please read the precautions on the back before filling in this education) — I1T ------ .. Zhang Zhiben fits a standard f centimeter 7 4195 31 Printed by the Consumer Standards Cooperative of the Central Bureau of Standards of the Ministry of Economic Affairs A7 B7 Invention Description (5) There is liquid seawater pumped through a pipeline and steam introduced into the shell side of the exchanger to heat the seawater. The seawater did not boil as it passed through the pipeline, as there was sufficient pressure in it to prevent it from bouncing. Then the hot seawater flowing out of the exchanger tube is transferred upward to the Shanghai water tank located above the heat exchanger. As the seawater flows upward, the pressure drops and the hot seawater boils, forming a two-phase mixture of concentrated seawater and water vapor. When the two-phase mixture enters the seawater tank, the water vapor is separated from the seawater, and leaves the seawater to the condenser 'during which the water vapor is condensed to form distilled water. The seawater is recovered to the evaporator by a circulating pump, and a part of it is removed downstream with seawater for further salt crystallization and recovery. Furthermore, when using a falling film evaporator, the feed water is added to the seawater tank or to the seawater loop. Although falling film and powerful circulation evaporators are generally used for water evaporation applications, their usability depends on the rate of formation and accumulation on the surface of the evaporator heat exchanger. The system is very important because the scale forming system on the surface of the device acts as an insulator and needs to be removed periodically in order to effectively operate the evaporator unit. The scale composition shown in Table 2 is formed by the evaporation of vaporized gray water. Among them, a falling film and a strong circulation evaporator are used in series. The main scale ingredients are silicon oxide (Si02), calcium fluoride (CaF2) and magnesium fluoride (MgF2). (Please read the notes on the back before filling this page)
本紙張尺度適用中國國家標準( 匚阳)八4規格(210\297公釐) 4 J95 31 A7 B7 經濟部中夾標準局員工消費合作社印装 五、發明説明(6 ) 第2表 丰排放丨水篆曼_形成之管線垢及槽垢之組成 鎮 (重量%) 矽 (重量%) 磷 (重量%) 硫 (it%) 鈣 (重量%) 鐵 (重量 強力循環蒸發器 管垢 91 2 2 0 3 2 強力循環蒸發器 槽垢 1 80 0 7 8 4 落膜蒸發器管垢 3 55 0 2 40 0 落琪蒸發器管垢 3 43 1 0 49 4 依據本發明’可藉由使水無機酸之水溶性鹽溶液(包 含其水合物)使氟化物垢自鈦、鈦合金、錄合金及不鏞鋼 移除。鹽類之陽離子部份可為鋁、離子或其混合。鹽類之 陰離子可為氯化物、硝酸鹽、硫酸鹽及其混合物。接觸係 發生於缺乏添加酸時,諸如,氫氯酸、硝酸或流酸。具有 溶解氟化物垢之水性鹽溶液之存在不會促進或增加金屬腐 钱之正常速率(其會發生於缺乏水性鹽溶液或任何清潔劑 )° 較佳之鹽類為由氯化铭、硫酸紹、琐酸銘及其水合物 及其混合物製成之鋁鹽溶液。硝酸鋁為較佳之鋁鹽,其中 被處理之裝置為部份氧化氣化系統之一部份,因所用之溶 液可回復至氣化系統,且對氣化器供料具有最少之衝擊。 硝酸鋁鹽之硝酸鹽组份變成合成氣體(如,、NH3或c〇) 之—部份。相對地,氯化鋁以氣化鋁型式添加氣化物至供 料,且硫酸鋁添加硫及硫酸鈣沈澱物於蒸發器内。 雖然無機酸之鐵鹽亦可被同於溶解氟化物垢,基於溶 本紙張碰賴(CNS) Α4&格(21QX297公廢)~ — ~ (請先閲讀背面之注意事項再填寫本頁)This paper size applies to the Chinese National Standard (Liyang) 8 4 specifications (210 \ 297 mm) 4 J95 31 A7 B7 Printed by the Consumer Cooperatives of the China National Standards Bureau of the Ministry of Economic Affairs 5. Description of the invention (6) Table 2 Feng emissions 丨Waterman_Composition of pipeline scale and tank scale formed town (wt%) silicon (wt%) phosphorus (wt%) sulfur (it%) calcium (wt%) iron (weight strong circulation evaporator tube scale 91 2 2 0 3 2 Powerful circulating evaporator tank scale 1 80 0 7 8 4 Falling film evaporator tube scale 3 55 0 2 40 0 Falling Qi evaporator tube scale 3 43 1 0 49 4 According to the present invention, the The water-soluble salt solution (including its hydrate) allows fluoride scale to be removed from titanium, titanium alloys, alloys, and stainless steels. The cationic portion of the salts can be aluminum, ions, or a mixture thereof. The anions of the salts can be Are chlorides, nitrates, sulfates, and mixtures thereof. Contact occurs in the absence of added acids, such as hydrochloric acid, nitric acid, or flowing acid. The presence of an aqueous salt solution with dissolved fluoride scale does not promote or increase metals Normal rate of money corruption (which occurs when there is a lack of (He cleaner) ° The preferred salts are aluminum salt solutions made of chlorinated salt, sulphuric acid salt, oxalic acid salt and their hydrates and their mixtures. Aluminum nitrate is the preferred aluminum salt, of which the device to be treated is As part of the oxidizing gasification system, the solution used can be returned to the gasification system with minimal impact on the gasifier feed. The nitrate component of aluminum nitrate becomes a synthesis gas (such as, NH3 or c〇)-Part. In contrast, aluminum chloride is added as a gasified aluminum to the feed, and aluminum sulfate is added with sulfur and calcium sulfate precipitates in the evaporator. Although iron salts of inorganic acids can also be used Same as dissolving fluoride scale, based on dissolving paper (CNS) Α4 & (21QX297 public waste) ~ — ~ (Please read the precautions on the back before filling this page)
4 195 3 1 經 中 央 橾 準 局 員 工 消 費 合 h 社 印 製 A7 B7 五、發明説明(7 ) 解氣化物垢及抑制酸溶液中鈦之說化物腐姓之莫耳比較基 礎上,鐵鹽一般不如鋁鹽有效。 無機酸之水性鹽溶液具有之濃度需為約1 %至約4 0 % ,較佳為約15°/。至約2〇% ,且溫度為約32卞至約212卞。若 溶液被加熱至約l〇〇°F至約212卞,較佳為約175卞至約212 F之/jnL度時,鹽溶液於溶解氟化物垢以速率及溶解量來 看更有效。於比較测試中,於1〇〇卞時於9〇分鐘内溶解之 垢能於175卞於1分鐘内溶解。 水性無機鹽溶液與垢表面接觸一足以有效移除或溶解 氟化物垢之時間,其一般為約3〇分鐘至約24小時,較佳為 約1小時至約3小時。無機鹽溶液之混合(包括其水合物之 溶液)可被使用之。水性鹽溶液之起始pH一般係至少約15 〇 在以無機酸之水性鋁鹽溶液處理金屬表面之前或後時 三鹼金屬氫氧北物之溶液(諸如,氫氧化鈉(Na〇H)或氫 乳化却(KOH)可被用於接觸及處理金屬表面以移除任何 氧化矽垢或氰化鐵垢。 鹼金屬氫氧化物處理(特別是Na0H處理)一般係被 選,第一垢清除溶液,主要係因為苛性溶液比鋁鹽溶液較 不印貝’特別是確酸铭溶液。 ‘鹼金屬氫氧化物溶液之濃度需為約1%至約25。/。,較 佳為約2%至6%,且需被加熱約170T至212eF之溫度,或 至於大氡力時溶液之沸點。鹼金屬氫氧化物溶液需與垢表 面接觸一足以有效移除氡化矽或氰化鐵垢之時間,其一般 為約30分鐘至約24小時,且較佳為約2小時至約6小時,氫 本纸張尺㈣财 (請先閱讀背面之注意事項再填寫本可,)4 195 3 1 A7 B7 printed by the Consumers ’Association of the Central Bureau of Standards and Assistance. 5. Description of the invention (7) On the basis of the comparison of Moore, which degasses the scale of the gas and inhibits the titanium in the acid solution, iron salts are generally not as good. Aluminum salts are effective. The aqueous salt solution of the inorganic acid has a concentration of about 1% to about 40%, preferably about 15 ° /. To about 20%, and the temperature is about 32 ° to about 212 °. If the solution is heated to a temperature of about 100 ° F to about 212 ° F, preferably about 175 ° F to about 212 ° F / jnL degrees, the salt solution is more effective in dissolving the fluoride scale in terms of rate and amount of dissolution. In a comparative test, scales that dissolve in 100 minutes at 100 hours can dissolve in 175 minutes in 1 minute. The time that the aqueous inorganic salt solution is in contact with the scale surface is sufficient to effectively remove or dissolve the fluoride scale, which is generally about 30 minutes to about 24 hours, preferably about 1 hour to about 3 hours. Mixtures of inorganic salt solutions (including solutions of their hydrates) can be used. The initial pH of an aqueous salt solution is generally at least about 15 °. A solution of a tribasic metal hydroxide (such as sodium hydroxide (NaOH) or sodium hydroxide) before or after treating the metal surface with an aqueous aluminum salt solution of an inorganic acid. Hydrogen emulsified (KOH) can be used to contact and treat metal surfaces to remove any oxidized silica scale or iron cyanide scale. Alkali metal hydroxide treatment (especially NaOH treatment) is generally selected as the first scale removal solution Mainly because the caustic solution is less imprinted than the aluminum salt solution, especially the acid solution. 'The concentration of the alkali metal hydroxide solution needs to be about 1% to about 25., preferably about 2% to 6%, and it needs to be heated at a temperature of about 170T to 212eF, or the boiling point of the solution at high pressure. The alkali hydroxide solution must be in contact with the scale surface for a time sufficient to effectively remove the silicide silicon or iron cyanide scale It is usually about 30 minutes to about 24 hours, and preferably about 2 hours to about 6 hours. Hydrogenated paper is not enough money (please read the precautions on the back before filling in this,)
10 4195 31 經濟部中央標準局—工消費合作社印製 Α7 Β7 五、發明説明(8 ) 氧化鈉或氫氧化鉀之混合物亦可被使用之β當自鈦移除垢 時’硝酸鈉抑制劑一般係與苛性物使用之。 於苛性清潔操作已完成後,在引入水性無機鹽溶液前 ’苛性溶液需自裝置移除,其係藉由,諸如,由其漸次排 出而達成之,反之亦滅。於每一清潔溶液移除後,無需特 別之清理《因此,下一清潔溶液(即,水性無機鹽溶液) 可以相似方式被引入裝置及被移除之。 氫氧化鈉之混合之所用之中和溶液及水性無機鹽溶液 可被混合,以水稀釋至約95%水之濃度且使用額外之氫氧 化鈉(若需要的話)中和至pH約為7。 然後,中和之用過之清潔溶液可被用於漿化原料(諸 如,煤)。以作為部份氧化反應。因此,例如,氟化物、 鈉、鋁及矽組份變成副產物礦渣之組份。若用過之驗溶液 被循環至氣化器,循環溶液需以小量添加至原料,以便不 會明顯增加鈉或鉀供料濃度,其對於氣化器之阻燃性内襯 具有不利作用。未中和之用途之鋁鹽溶液可被循環至氣化 器供枓,只要其與原料以一夠低速率摻合,以便原料之pH 值不低於6, Ο β 需注意藉由使用無驗之水性鹽溶液,以替代使用具添 加鋁鹽之無機酸清潔溶液,清潔方法不會加速腐蝕或增加 腐蝕速率,然而,使用酸時,需小心添加足夠鋁抑制劑以 降低或停止加速腐蝕。因為清理前裝置内之垢含量不被真 正獲知且對於保存化學清潔溶液具經濟需求,此為重要考 量0 測定是否需更多滑潔溶液添加至裝置之裝置可藉由媳 本紙張尺度適用中國國家標準(CNS ) A4規格(2〗Οχ29?公釐) f請先閲讀背面之注意事項再填寫本頁)10 4195 31 Printed by the Central Bureau of Standards of the Ministry of Economic Affairs—Industrial and Consumer Cooperatives A7 B7 V. Description of the invention (8) Mixtures of sodium oxide or potassium hydroxide can also be used. Β When removing scale from titanium, sodium nitrate inhibitors are generally used. Used with caustics. After the caustic cleaning operation has been completed, the caustic solution needs to be removed from the device before the aqueous inorganic salt solution is introduced, which is achieved, for example, by its gradual discharge, and vice versa. After each cleaning solution is removed, no special cleaning is required. Therefore, the next cleaning solution (ie, the aqueous inorganic salt solution) can be introduced into the device and removed in a similar manner. The neutralizing solution used for the mixing of sodium hydroxide and the aqueous inorganic salt solution can be mixed, diluted with water to a concentration of about 95% water and neutralized with additional sodium hydroxide (if necessary) to a pH of about 7. The used cleaning solution for neutralization can then be used to slurry raw materials (e.g., coal). As a partial oxidation reaction. Thus, for example, the fluoride, sodium, aluminum, and silicon components become components of the by-product slag. If the used test solution is recycled to the gasifier, the recycled solution needs to be added to the raw material in a small amount so as not to significantly increase the sodium or potassium feed concentration, which has an adverse effect on the flame retardant lining of the gasifier. The aluminum salt solution for non-neutralizing purposes can be recycled to the gasifier for supply, as long as it is blended with the raw material at a low enough rate so that the pH value of the raw material is not lower than 6, Ο β Instead of using an inorganic acid cleaning solution with an aluminum salt, the cleaning method will not accelerate corrosion or increase the corrosion rate. However, when using an acid, be careful to add enough aluminum inhibitor to reduce or stop accelerated corrosion. Because the scale content in the device before cleaning is not really known and there is an economic need for storing chemical cleaning solutions, this is an important consideration. 0 The device that determines whether more slip cleaning solution is added to the device can be applied to the country of China by the size of the paper Standard (CNS) A4 specification (2〗 〇χ29? Mm) f Please read the notes on the back before filling in this page)
11 4 195 31 經濟部中央標準局員工消費合作社印製 A7 B7 五、發明説明(9 ) 固體刀析决疋之,其中過渡清潔溶液由被處理之裝置取出 且於105°C乾燥,並測量殘質重量β 起始β潔溶液及與垢相接觸之清潔溶液之總溶解固體 濃度可被用於決定清潔溶液是否以垢化合物飽和之。氧化 矽對鹼氫氧化物莫耳比例〇·5及氟化鈣對鋁鹽溶液之莫耳 比例0.65需被用於決定清潔溶液之飽和點。此方式中,所 用清潔溶液之量可被減少之。 於範例中及整件說明書,除非有其它表示,所有濃度 係為重量%。 範例1 -6 表1中之組成之排放水於落膜蒸發器内蒸發產生水蒸 氣與海水之混合物。混合物被饋入落膜蒸發器之海水槽, 其間水蒸氣與海水分離之且被饋入冷凝器以回收水蒸餾液 。於操作蒸發器約42天後,垢於蒸發器管線内側之鈦表面 及HastelloyTM c_276 (Haynes Metals c〇)高鎳合金(其形 成槽)之表面上發展。 垢藉由自表面剝離薄片自海水槽之金屬表面及藉由以 槌子衝擊鈦管線之外侧自蒸發器管線機械式移除。垢之組 成為約50%非晶型氧化矽及50%氟化鈣。分離6克之垢樣 品係於170T起始與100克之具有濃度為6%或之氫氧化 鈉溶液接觸至少2小時。於處理期間後,苛性溶液藉由 Inductively Coupled Plasma (ICP)儀器方法分析氯化物之 金屬及離子之色譜及以苛性溶液溶解之Si、Ca及F之重量 被測定。 垢樣品與pH值為1〜2且溫度為1〇〇卞之硝酸鋁溶液接 本紙張尺度適用中國國家標準(CNS ) A4規格(210X297公釐) 12 (請先閲讀背面之注意事項再填寫本頁}11 4 195 31 Printed by the Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the invention (9) The analysis of the solid knife is made, in which the transition cleaning solution is taken out from the treated device and dried at 105 ° C, and the residual The mass concentration of the starting β cleaning solution and the total dissolved solids concentration of the cleaning solution in contact with scale can be used to determine whether the cleaning solution is saturated with scale compounds. The molar ratio of silicon oxide to alkali hydroxide 0.5 and the molar ratio of calcium fluoride to aluminum salt solution 0.65 need to be used to determine the saturation point of the cleaning solution. In this way, the amount of cleaning solution used can be reduced. In the examples and throughout the specification, all concentrations are% by weight unless otherwise indicated. Example 1 -6 The discharged water of the composition in Table 1 is evaporated in a falling film evaporator to produce a mixture of water vapor and sea water. The mixture is fed into the seawater tank of the falling film evaporator, during which water vapor is separated from the seawater and fed into the condenser to recover the water distillate. After operating the evaporator for approximately 42 days, scale developed on the titanium surface inside the evaporator line and on the surface of HastelloyTM c_276 (Haynes Metals c) high nickel alloy (which forms the groove). Scale was removed from the metal surface of the seawater tank by peeling the sheet from the surface and mechanically removed from the evaporator line by striking the outside of the titanium line with a mallet. The scale group becomes about 50% amorphous silicon oxide and 50% calcium fluoride. Six grams of scale samples were separated at the beginning of 170T and contacted with 100 grams of a sodium hydroxide solution having a concentration of 6% or at least 2 hours. After the treatment period, the caustic solution was analyzed by chromatographic analysis of chloride metals and ions and the weight of Si, Ca, and F dissolved in the caustic solution by an Inductively Coupled Plasma (ICP) instrument method. The scale sample is connected to an aluminum nitrate solution with a pH value of 1 ~ 2 and a temperature of 100 ° C. The paper size applies the Chinese National Standard (CNS) A4 specification (210X297 mm) 12 (Please read the precautions on the back before filling in this page}
4195 31 Α7 Β7 五、發明説明(10 ) (請先閱讀背面之注意事項再填寫本頁) 觸至少2小時。於範例4〜6中,硝酸鋁溶液亦含有0,5或1 .〇〇/〇 之硝酸納(NaN〇3) ’其被用以抑制鈦中之水合物相之形成 。於處理期間後,硝酸鋁溶液以Icp方法分析氟化物之金 屬及離子之色譜,且以硝酸鋁溶解之Si、Ca&F之重量被 測定之^範例顯示含有垢之氟化物使用硝酸鋁溶液有效移 除,其於範例1,4及6中具有超過90%之垢移除。結果係 記錄於第3表中,如下所示: 第3表 落媒蒸發器槽垢之移除 範例 溶液 苛性處理 時間 (小時) 溫度 (°F) 溶解以 (起始垢 重量之 溶解之Ca (起始垢 重量之%) 溶^1F (起始垢 重量之%) 溶解Si對 清潔溶液 中之NaOH 之莫耳比 率 1 6%NaOH-U.2°/〇 ΑΚΝΟ^ 2 170 30 0 3 0.43 2 6%NaOH-11.2% AJ(N〇A 2.5 170 20 0 1.5 029 3 10% NaOH (l%NaNQ3> U.2%AI(NQj)3 4 170 7.7 0 3.7 0.64 4 10% NaOH (I%NaN〇3> 16%Α1(Ν03)3 5.3 170 10 0 5.5 0.089 5 10%NaOH (0.5 %NdNQ〇-12%準⑽ 5.8 170 9.1 0 3.7 0.097 6 10%NaOH (0.5 VoNaNOO-mAlCNO^ 170 7.6 0 3.6 0.086 _本 經濟部中央標準局員工消費合作社印製 註:NaOH溶液之最大容量溶於每莫耳!^〇只為〇 5莫耳之沿(形成丨莫耳矽酸 鈉需2。莫耳NaOH)。當Si對NaOH之比例為0.5時,溶液被完全利用之。 於100 F時Α1(Ν〇3)3溶液之最大容量被溶於每莫耳鋁為約13莫耳之氟化 物(0.65莫耳CaF2)(於Ca^溶解測試事先測定當氟化物對鋁之比例 為1.3或故化物對NO3之比例為0.43時’溶液被完全使用a s174»F時, 對於每莫耳之銘,1.6莫耳之氟化物((^莫耳^^^)被溶解。 國家橾準(CNS ) Μ規格(210X297公釐) 4 195 31 A7 B7 五、發明説明(11 ) 第3表(績)落膜蒸發器槽垢之移除 範例 溶液 硝酸鹽處理 時間 (小時) 溫度 (°F) 溶解之Si (起始垢 重量之%) 溶解之Ca (起始垢 重量之%) 溶解之F (起始垢 重量之%) 溶解Si對 清潔溶液 中之NaOH 之莫耳比 率 I 6%NaOH-11.2% AKNO^ 2 100 0.4 15 15 028 2 6%NaOH-11.2% AI(N03)3 6.3 100 0.1 21 14 026 3 10%.NaOH (l%NaN〇3>-11.2%Α1(ΝΟ^ 4 100 03 22 17 0.32 4 10% NaOH (l0/〇NaNO3)- 16%Al(N〇3)3 6 100 0 25 27 0.33 5 10%NaOH (0.5 %NaNO> 12%Al(N〇3)3 3.5 170 0.2 21 22 0.2S 6 10% NaOH (0.5 %NaN03)-Ιβ%Α1(ΝΟ^ 1 [70 0.2 21 18 0.26 (請先閲讀背面之注意事項再填寫本頁) 經濟部中央標準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(210 X 297公釐) 14 419531 A7 B7 五、發明説明(ί2 ) 第3表(續) 落膜蒸發器槽垢之移除 範例 描述 殘質組成 苛性清理後之 殘質1 起始垢重量 之% 落膜蒸發器槽 垢之移除, 起始垢重量 之% SI 〇 Ca F A1 I 6%NaOH-li.2% ΑΚΝΟΛ 51 8 37 51 4 0 - 2 6%NaOH-I1.2% 雖姑 55 72* 55 53 6 0 - 3 10% NaOH (l%NaN03> — 20** 8 0 50 23 — 4 10% NaOH (l%NaN〇3)- AliNO^ 73 6 31 46 1 0 - 5 10% NaOH (0,5 %NaN〇3> 12%AJ(N03)3 71 21*料 14 30 I 22 29 6 10% NaOH (0.5 %NaN〇3> I6%AI(N03)3 74 7*** 6 30 4 26 26 *範例2之殘質可使用新的Α〖(Ν03)3及NaOH溶液進一步持續清理至所有垢被 完全溶解為止。下列結果被獲得之且以溶液濃度、時間、溫度及清理後之百 分率殘質之連續順序表示,第三清理-11.2% A1(N03)3-3小時-14% ;第四清理 -11.2% Al(N〇3)3-6小時-13% ;第五清理-2% NaOH-2小時-6% ;第六清理-6% NaOH-1.5小時完全溶解垢。 _範例3之殘質被接受170下時之3.2克之10%此011-1%此船35.5小時,殘質 降至12% (此殘質之主要组份為CaF2)。 木林X-射線衍射分析顯示殘質主要含A12(0H)3F3。 11... II (請先閱讀背面之注意事項再填寫本頁) 訂 經濟部中央標準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(210X 297公釐) 15 4IS5 3i Α7 Β7 五、發明説明(13 ) 範例9 二水溶性(“A”及“B”)被製成含有1%之氟化物( 由氟化鈣粉末)及4%氯化鋁(為腐蝕抑制劑)<3 1%濃度 之氫氯酸亦被添加至溶液A。二溶液被加熱至1〇〇卞且與 第2等級之鈦接觸24小時。腐蝕速率及其它資料被記錄於 第4表。 第4表 HC1 濃度 溶液pH值 (起始) 溶液pH值 (最終) 鈦腐蝕速率 (密耳/年) ~63M ---~~~-. 溶液A 1% 0.3 0.4 溶液B ---—---- 2.7 ~~ ------ 3.3 (請先閱讀背面之注意事項再填寫本頁} V pkm tKH k __I本 經濟部中央標準局貝工消費合作社印製 於約5密耳/年。溶液A之腐钱逮率非常高且會造成^ 金屬損失。其證實當使用酸清理欽產生之B㈣時 用酸溶液溶解氟化物垢’即使以腐蝕抑制劑,會 吏 腐蝕。 取重大 使周酸清潔劑之問題為單元内氣化物垢之量於 係未知。因此,鋁腐蝕抑制劑之量 曰則 =率;=一’氟化物垢被溶解且二 “4 規格⑺“公瘦' ----訂-- rI. 16 _4195 31 Α7 Β7 V. Description of the invention (10) (Please read the precautions on the back before filling this page) Touch for at least 2 hours. In Examples 4 to 6, the aluminum nitrate solution also contains sodium nitrate (NaNO3) ', which is used to inhibit the formation of a hydrate phase in titanium. After the treatment period, the aluminum nitrate solution was analyzed by Icp method for fluoride metal and ion chromatography, and the weight of Si, Ca & F dissolved in aluminum nitrate was measured. Examples show that scale-containing fluoride is effective with aluminum nitrate solution. Removal, which has more than 90% scale removal in Examples 1, 4 and 6. The results are recorded in Table 3, as shown below: Table 3 Example of removal of scale from falling evaporator evaporator Caustic treatment time (hours) Temperature (° F) Dissolved with (Ca. % By weight of starting scale) Soluble ^ 1F (% by weight of starting scale) Molar ratio of dissolved Si to NaOH in the cleaning solution 16.6% NaOH-U.2 ° / 〇ΑΚΝΟ ^ 2 170 30 0 3 0.43 2 6% NaOH-11.2% AJ (N〇A 2.5 170 20 0 1.5 029 3 10% NaOH (l% NaNQ3 > U.2% AI (NQj) 3 4 170 7.7 0 3.7 0.64 4 10% NaOH (I% NaN. 3 > 16% Α1 (Ν03) 3 5.3 170 10 0 5.5 0.089 5 10% NaOH (0.5% NdNQ〇-12% standard) 5.8 170 9.1 0 3.7 0.097 6 10% NaOH (0.5 VoNaNOO-mAlCNO ^ 170 7.6 0 3.6 0.086 _ Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs Note: The maximum capacity of NaOH solution is soluble per mole! ^ 〇 is only 0. 5 Moore's edge (2 Molar NaOH is required to form sodium silicate). When the ratio of Si to NaOH is 0.5, the solution is fully utilized. At 100 F, the maximum capacity of the A1 (NO3) 3 solution is dissolved in about 13 moles of fluoride per mole of aluminum (0.65 moles). Ear CaF2) (in Ca ^ dissolution test First, when the ratio of fluoride to aluminum is 1.3 or the ratio of chemical compounds to NO3 is 0.43, when the solution is completely used as s174 »F, 1.6 mol of fluoride ((^ mol ^^^) is dissolved. National Standards (CNS) M specifications (210X297 mm) 4 195 31 A7 B7 V. Description of the invention (11) Table 3 (achievement) Example of removal of scale from falling film evaporator solution nitric acid Salt treatment time (hours) Temperature (° F) Dissolved Si (% of initial scale weight) Dissolved Ca (% of initial scale weight) Dissolved F (% of initial scale weight) Dissolved Si in cleaning solution Molar ratio of NaOH I 6% NaOH-11.2% AKNO ^ 2 100 0.4 15 15 028 2 6% NaOH-11.2% AI (N03) 3 6.3 100 0.1 21 14 026 3 10%. NaOH (l% NaN〇3 > -11.2% Α1 (ΝΟ ^ 4 100 03 22 17 0.32 4 10% NaOH (l0 / 〇NaNO3)-16% Al (N〇3) 3 6 100 0 25 27 0.33 5 10% NaOH (0.5% NaNO > 12 % Al (N〇3) 3 3.5 170 0.2 21 22 0.2S 6 10% NaOH (0.5% NaN03) -Ιβ% Α1 (ΝΟ ^ 1 [70 0.2 21 18 0.26 (Please read the notes on the back before filling this page ) Printed by the Consumer Cooperatives of the Central Standards Bureau of the Ministry of Economic Affairs Standards are applicable to Chinese National Standard (CNS) A4 specifications (210 X 297 mm) 14 419531 A7 B7 V. Description of the invention (2) Table 3 (continued) Example of removal of scale from falling film evaporator Description of caustic cleaning of residual components Residual residue 1% of initial scale weight Removal of falling scale from falling film evaporator,% of initial scale weight SI 〇Ca F A1 I 6% NaOH-li.2% ΑΚΝΟΛ 51 8 37 51 4 0-2 6% NaOH-I1.2% Although it is 55 72 * 55 53 6 0-3 10% NaOH (l% NaN03 > — 20 ** 8 0 50 23 — 4 10% NaOH (l% NaN〇3)-AliNO ^ 73 6 31 46 1 0-5 10% NaOH (0.5% NaN〇3> 12% AJ (N03) 3 71 21 * material 14 30 I 22 29 6 10% NaOH (0.5% NaN〇3> I6% AI (N03) 3 74 7 *** 6 30 4 26 26 * The residue of Example 2 can be further cleaned continuously with new A ((N03) 3 and NaOH solution until all scales are completely dissolved. The following results were obtained and expressed in a continuous order of solution concentration, time, temperature, and percentage residues after cleaning, the third cleaning -11.2% A1 (N03) 3-3 hours -14%; the fourth cleaning -11.2% Al (N03) 3-6 hours -13%; fifth cleaning-2% NaOH-2 hours-6%; sixth cleaning-6% NaOH-1.5 hours completely dissolved scale. _ The residue of Example 3 is 10% of 3.2 grams at 170 times, the 011-1% of this ship is 35.5 hours, and the residue is reduced to 12% (the main component of this residue is CaF2). X-ray diffraction analysis of Mulin showed that the residue mainly contained A12 (0H) 3F3. 11 ... II (Please read the precautions on the back before filling out this page) Order printed by the Central Consumers Bureau of the Ministry of Economic Affairs, printed by the Consumer Cooperatives. The paper size applies to the Chinese National Standard (CNS) A4 (210X 297 mm) 15 4IS5 3i Α7 Β7 V. Description of the invention (13) Example 9 Two water-soluble ("A" and "B") are made containing 1% fluoride (from calcium fluoride powder) and 4% aluminum chloride (for corrosion inhibitors) ) ≪ 3 1% hydrochloric acid was also added to solution A. The two solutions were heated to 100 ° F and contacted with Ti grade 2 titanium for 24 hours. Corrosion rates and other information are recorded in Table 4. Table 4 HC1 Concentration Solution pH (Initial) Solution pH (Final) Titanium Corrosion Rate (mils / year) ~ 63M --- ~~~-. Solution A 1% 0.3 0.4 Solution B ------ --- 2.7 ~~ ------ 3.3 (Please read the notes on the back before filling out this page} V pkm tKH k __I This is printed by the Shellfish Consumer Cooperative of the Central Standards Bureau of the Ministry of Economic Affairs at about 5 mils / year The corrosion rate of solution A is very high and can cause metal loss. It proves that when using acid to clean up the B㈣ produced by acid, the acid solution is used to dissolve the fluoride scale, even if it is a corrosion inhibitor, it will corrode. The problem with acid cleaners is that the amount of gaseous scale in the unit is unknown. Therefore, the amount of aluminum corrosion inhibitor is = rate; = one 'fluoride scale is dissolved and two "4 specifications" "male thin"- --Order-- rI. 16 _
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