TW201726231A - Processing method of formic acid and processing device of formic acid capable of processing formic acid in mass and reducing concentration of formic acid below 0.5 volume ppm - Google Patents
Processing method of formic acid and processing device of formic acid capable of processing formic acid in mass and reducing concentration of formic acid below 0.5 volume ppm Download PDFInfo
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本發明係關於一種藉由乾式處理使包含甲酸蒸汽之氣體無害化之方法及裝置。The present invention relates to a method and apparatus for detoxifying a gas comprising formic acid vapor by dry treatment.
甲酸被使用於農業、纖維工業、有機合成化學、半導體裝置製造業等廣泛之領域。近年來,於真空回流焊接裝置中,為了將焊料表面之氧化物還原,而開發出使用甲酸之方法,且該方法不斷迅速發展。通常,真空回流焊接裝置之排氣包含1體積%以上之甲酸。然而,甲酸蒸汽對眼睛及皮膚有害,推薦之暴露容許濃度(TLV)為5體積ppm。因此,包含甲酸蒸汽之氣體於排放至大氣中之前,需要進行無害化處理。進而,為了防止由甲酸所引起之配管腐蝕或防止周邊環境之惡臭,而要求進一步降低排氣中之甲酸濃度,例如降低至0.5體積ppm以下。 到目前為止,作為排氣中之甲酸蒸汽之處理方法,有使其於燃燒器中流通而進行燃燒除害之方法、於觸媒存在下加熱而進行熱分解處理之方法、或不使用觸媒而加熱至200℃以上進行熱分解處理之方法(專利文獻1),但均需要大型裝置,妨礙小規模從業者引進真空回流焊接裝置。 又,作為甲酸蒸汽之處理方法,亦有使包含甲酸蒸汽之排氣與水或醇接觸而使甲酸溶解而進行濕式處理之方法(專利文獻2),但需要大型裝置及廢液處理,進而若水溶液中之甲酸濃度超過90質量%則相當於劇毒物,因而亦存在廢液處理受到限制之情形,仍然不適於小規模從業者。 作為易處理之酸性氣體之除害方法,已知有利用對固體之吸附之乾式處理方法。例如,作為硫氧化物、氯化氫等酸性氣體之乾式處理方法,廣泛使用鹼金屬或鹼土金屬之氫氧化物,自成本及處理之容易性考慮,主要使用氫氧化鈣(專利文獻3)。作為以鹵素系氣體及酸性氣體為處理對象之示例,可列舉包含熟石灰之造粒體之吸附劑(專利文獻4)、或以氧化性氣體及酸性氣體為處理對象之包含鹼石灰、沸石及活性碳之混合物之造粒體之處理劑(專利文獻5)等。於專利文獻5中,於實施例及比較例中雖然對甲酸蒸汽進行處理,但並未處理至TLV以下。又,使用含有K2 CO3 之活性碳,將氣體中之甲酸蒸汽之濃度自100 ppm處理至10 ppm(專利文獻6)。 乾式處理中所使用之固體材料藉由物理吸附或化學吸附將氣體中所包含之酸性氣體固定而自氣體中去除。物理吸附係酸性氣體藉由范德華力吸附於固體材料之狀態,其結合較弱,於溫度或壓力之控制下可逆地產生吸附、脫離。化學吸附係酸性氣體藉由化學反應而與固體材料吸附之狀態,其結合牢固,氣體一旦吸附很難脫離。 [先前技術文獻] [專利文獻] [專利文獻1]日本專利特開2007-125578號公報 [專利文獻2]日本專利特開2001-244618號公報 [專利文獻3]日本專利特開2002-029738號公報 [專利文獻4]日本專利特開2005-177576號公報 [專利文獻5]日本專利特開2004-181300號公報 [專利文獻6]日本專利特開平9-86914號公報Formic acid is used in a wide range of fields such as agriculture, fiber industry, organic synthetic chemistry, and semiconductor device manufacturing. In recent years, in a vacuum reflow soldering apparatus, a method of using formic acid has been developed in order to reduce an oxide on a solder surface, and the method has been rapidly developed. Usually, the exhaust gas of the vacuum reflow soldering apparatus contains 1% by volume or more of formic acid. However, formic acid vapor is harmful to the eyes and skin, and the recommended exposure allowable concentration (TLV) is 5 ppm by volume. Therefore, the gas containing formic acid vapor needs to be detoxified before being discharged into the atmosphere. Further, in order to prevent corrosion of piping caused by formic acid or to prevent odor of the surrounding environment, it is required to further reduce the concentration of formic acid in the exhaust gas, for example, to 0.5 ppm by volume or less. Heretofore, as a method of treating formic acid vapor in the exhaust gas, there is a method of circulating it in a burner to perform combustion and detoxification, a method of performing thermal decomposition treatment by heating in the presence of a catalyst, or a catalyst is not used. On the other hand, a method of performing thermal decomposition treatment at a temperature of 200 ° C or higher (Patent Document 1) requires a large-scale apparatus and prevents a small-scale practitioner from introducing a vacuum reflow soldering apparatus. Further, as a method of treating formic acid vapor, there is a method in which a formic acid vapor-containing exhaust gas is brought into contact with water or an alcohol to dissolve the formic acid and is subjected to a wet treatment (Patent Document 2), but a large-scale apparatus and waste liquid treatment are required, and further If the concentration of formic acid in the aqueous solution exceeds 90% by mass, it is equivalent to a highly toxic substance, and thus there is a case where the disposal of the waste liquid is restricted, and it is still unsuitable for a small-scale practitioner. As a method for detoxifying a manageable acid gas, a dry treatment method using adsorption to a solid is known. For example, as a dry treatment method of an acid gas such as sulfur oxide or hydrogen chloride, a hydroxide of an alkali metal or an alkaline earth metal is widely used, and calcium hydroxide is mainly used in view of cost and ease of handling (Patent Document 3). Examples of the object to be treated by the halogen-based gas and the acid gas include an adsorbent containing granules of slaked lime (Patent Document 4), or an alkali hydrate, zeolite, and active agent treated with an oxidizing gas and an acid gas. A treatment agent for granules of a mixture of carbon (Patent Document 5) and the like. In Patent Document 5, in the examples and the comparative examples, formic acid vapor was treated, but it was not treated to TLV or less. Further, the concentration of the formic acid vapor in the gas was treated from 100 ppm to 10 ppm using activated carbon containing K 2 CO 3 (Patent Document 6). The solid material used in the dry treatment is removed from the gas by physical adsorption or chemical adsorption to fix the acid gas contained in the gas. The physical adsorption system acid gas is adsorbed to the solid material by van der Waals force, and the combination is weak, and reversibly generates adsorption and detachment under the control of temperature or pressure. The chemical adsorption is a state in which the acid gas is adsorbed by the chemical reaction and the solid material is bonded, and the gas is firmly bonded, and the gas is hard to be detached once adsorbed. [PRIOR ART DOCUMENT] [Patent Document 1] Japanese Patent Laid-Open Publication No. JP-A No. 2001-257618 (Patent Document 2) Japanese Patent Laid-Open No. 2001-244618 (Patent Document 3) Japanese Patent Laid-Open No. 2002-029738 [Patent Document 4] Japanese Patent Laid-Open Publication No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei.
[發明所欲解決之問題] 然而,本發明者等人對各種已有處理劑進行研究,結果存在排氣氣體中之甲酸之處理量不充分之情況、或難以使排氣氣體中之甲酸濃度降低至0.5體積ppm以下之問題。 於如專利文獻3及4所記載之僅使用氫氧化鈣作為排氣氣體之處理劑之情形時,若使含有濃度數體積%之高濃度之甲酸之氣體流通,則可見不充分地吸附甲酸,而立即穿透吸附材料之現象。 進而,於如專利文獻5所記載之使用組合有活性碳與鹼石灰之處理劑之情形時,若使含有高濃度之甲酸之氣體流通,則雖然可於一定程度上吸附甲酸,但處理後之排氣氣體中之甲酸濃度超過0.5體積ppm。 本發明之目的在於提供一種甲酸之乾式處理方法,其即便通入包含甲酸蒸汽之氣體,與先前之處理劑相比亦能夠對大量之甲酸進行處理,並且使處理後之甲酸濃度降低至0.5體積ppm以下。 [解決問題之技術手段] 本發明者等人為了解決上述問題而反覆進行銳意研究,結果發現:利用併用碳質吸附劑與氫氧化鈣之處理劑對包含甲酸蒸汽之氣體進行一次處理後,使用多孔質吸附劑進行二次處理,藉此能夠增加處理劑之每單位體積之處理量,進而能夠去除甲酸而使甲酸濃度降低至0.5體積ppm以下,從而完成本發明。 即,本發明提供一種甲酸之處理方法,其係自包含甲酸之氣體中去除甲酸者,且包括:第一處理步驟,其係使用包含碳質吸附劑及氫氧化鈣之第一處理劑對上述氣體中所包含之甲酸進行處理;及第二處理步驟,其係進而使用多孔質吸附劑對上述第一處理步驟後之氣體進行處理。 [發明之效果] 藉由本發明,可提供一種甲酸之乾式處理方法,其即便通入包含甲酸蒸汽之氣體,與先前之處理劑相比亦能夠對大量之甲酸進行處理,並且使甲酸濃度降低至0.5體積ppm以下。[Problems to be Solved by the Invention] However, the inventors of the present invention have studied various conventional treating agents, and as a result, there is a case where the amount of formic acid in the exhaust gas is insufficiently processed, or it is difficult to make the formic acid concentration in the exhaust gas. Reduce the problem to below 0.5 ppm by volume. In the case where only calcium hydroxide is used as the treatment agent for the exhaust gas described in Patent Documents 3 and 4, when a gas containing a high concentration of formic acid having a concentration of several vol% is circulated, it is observed that the formic acid is not sufficiently adsorbed. The phenomenon of immediately penetrating the adsorbent material. Further, when a treatment agent containing activated carbon and soda lime is used as described in Patent Document 5, if a gas containing a high concentration of formic acid is circulated, the formic acid can be adsorbed to some extent, but after treatment, The concentration of formic acid in the exhaust gas exceeds 0.5 volume ppm. It is an object of the present invention to provide a dry treatment method for formic acid which is capable of treating a large amount of formic acid and reducing the concentration of formic acid after treatment to 0.5 volume even if a gas containing formic acid vapor is introduced into the gas. Below ppm. [Means for Solving the Problems] The inventors of the present invention have conducted intensive studies in order to solve the above problems, and as a result, found that a gas containing formic acid vapor is once treated by using a carbonaceous adsorbent and a treatment agent of calcium hydroxide in combination, and then used. The porous adsorbent is subjected to secondary treatment, whereby the amount of the treatment agent per unit volume can be increased, and the formic acid can be removed to reduce the formic acid concentration to 0.5 ppm by volume or less. That is, the present invention provides a method for treating formic acid, which is for removing formic acid from a gas containing formic acid, and comprising: a first treatment step of using a first treatment agent comprising a carbonaceous adsorbent and calcium hydroxide; The formic acid contained in the gas is treated; and a second treatment step is followed by treating the gas after the first treatment step using a porous adsorbent. [Effects of the Invention] According to the present invention, it is possible to provide a dry treatment method of formic acid which can treat a large amount of formic acid and reduce the concentration of formic acid to a level as compared with the prior treatment agent even if a gas containing formic acid vapor is introduced. 0.5 volume ppm or less.
以下,基於圖式對本發明之實施形態進行說明。圖1係表示本發明之甲酸處理裝置11之圖。甲酸處理裝置11具有:第一處理部13,其對來自甲酸使用裝置17之排氣氣體進行處理;及第二處理部15,其對經第一處理部13處理之氣體進一步進行處理。第一處理部13與第二處理部15分別包含具有氣體入口及氣體出口之處理劑填充容器。 再者,甲酸處理裝置11進行處理之排氣中所包含之甲酸濃度並無特別限定,但通常至少超過作為TLV之5體積ppm。又,甲酸處理裝置11亦能夠對甲酸濃度為1體積%以上之氣體進行處理。另一方面,甲酸處理裝置11進行處理之排氣中所包含之甲酸濃度通常被認為在10體積%以下。但是,根據本發明之方法,上限並無特別限定,實用上亦可為20體積%左右。 甲酸處理裝置11進行處理之排氣並非100%之甲酸蒸汽,而是包含特定濃度之甲酸之氣體。作為構成排氣之甲酸以外之氣體,不僅為空氣,亦考慮為氮氣或氬氣、氖氣、氦氣等惰性氣體,或者氫氣或一氧化碳氣體等還原性氣體,或者該等混合而成者。 於第一處理部13中,排氣氣體與第一處理劑接觸,排氣氣體中之甲酸藉由第一處理劑而被去除。例如,第一處理部13為內部填充有第一處理劑之管狀反應器等。再者,第一處理部13內亦可設有使氣體均勻之攪拌翼或隔板。 第一處理部與第二處理部無需特別加熱。又,於第一處理部與第二處理部中,所導入之排氣氣體之溫度較佳為0~100℃,通常為常溫附近。 第一處理劑包含碳質吸附劑及氫氧化鈣。作為碳質吸附劑,只要為多孔質之碳材料,則無特別限定,但其BET比表面積較佳為500 m2
/g以上,更佳為1000 m2
/g以上,進而較佳為1500 m2
/g。例如,作為碳質吸附劑,可使用活性碳。再者,作為活性碳,可使用包含金屬成分之活性碳,即所謂添加有金屬之活性碳,例如可使用添加有氧化銅及氧化鋅之活性碳。添加有金屬之活性碳於活性碳表面附著有金屬或其化合物,金屬相對於活性碳之濃度以金屬換算計為1~10質量%左右。 第一處理劑較佳為使用鹼石灰作為包含氫氧化鈣之材料。鹼石灰亦稱為蘇打石灰,係以氫氧化鈣作為主成分且包含鹼金屬氫氧化物及水分之材料。鹼石灰較佳為包含50質量%以上之氫氧化鈣,更佳為包含70質量%以上。作為鹼石灰,可使用粒徑為100 μm~5 mm且比表面積為1~100 m2
/g左右之粉狀或粒狀者。 第一處理劑只要包含氫氧化鈣及碳質吸附劑兩者,則形態並無特別限定,可使用氫氧化鈣與碳質吸附劑之混合品。第一處理劑中所包含之氫氧化鈣與碳質吸附劑之比率以質量比計,較佳為氫氧化鈣:碳質吸附劑=1:0.1~0.5,更佳為1:0.2~0.4。 於第一處理步驟中,藉由併用氫氧化鈣與碳質吸附劑,相較於分別單獨使用氫氧化鈣與碳質吸附劑,更能夠對大量之甲酸進行處理。氫氧化鈣可與甲酸反應生成甲酸鈣而使甲酸固定於處理劑,但由於其反應速度緩慢,故而於通常之排氣氣體之滯留時間內,僅有一部分氫氧化鈣得到有效利用。進而,碳質吸附劑可藉由物理吸附而將氣體狀之甲酸保持於孔隙中,其每單位體積之吸附量不及能夠以甲酸鈣之形式固定之氫氧化鈣。藉由併用氫氧化鈣與碳質吸附劑,首先由吸附速度較快之碳質吸附劑吸附甲酸,其後氫氧化鈣將自碳質吸附劑中緩緩釋出之甲酸固定,因此認為能夠吸附大量之甲酸。 又,氫氧化鈣化學吸附甲酸而以甲酸鈣之形式固定,因此使用後之處理劑亦不會向大氣中釋出甲酸,於處理劑之更換作業中甲酸不會自使用後之處理劑中漏出。進而,氫氧化鈣即便吸濕而吸附能力亦不會減弱,因此即便入口氣體中含有水分,即便對環境中之水分進行吸濕亦不會產生問題。 於第二處理部15中,第一處理部13之出口氣體與多孔質吸附劑接觸,出口氣體中之甲酸藉由多孔質吸附劑而被去除。例如,第二處理部15為內部填充有多孔質吸附劑之管狀反應器等。再者,第二處理部15內亦可設有使氣體之組成均勻之攪拌翼或隔板。 多孔質吸附劑只要為能夠物理吸附甲酸且比表面積較高之多孔質材料,則無特別限定,可使用碳質吸附劑或無機系吸附劑,具體而言,可使用活性碳或沸石、矽膠。 作為可用作多孔質吸附劑之沸石、矽膠,其BET比表面積較佳為100 m2
/g以上,更佳為200 m2
/g以上,進而較佳為300 m2
/g以上。例如,作為沸石,可使用A型、B型、X型、Y型等各種結構之沸石。再者,於使用沸石之情形時,亦可於沸石中添加pH指示劑。可根據伴隨甲酸之吸附之pH指示劑之變色,藉由目視確認沸石之pH,從而可確認更換時期。 用作多孔質吸附劑之活性碳之BET比表面積較佳為500 m2
/g以上,更佳為1000 m2
/g以上,進而較佳為1500 m2
/g。再者,作為活性碳,為了易於吸附作為酸性氣體之甲酸,可使用添加有金屬成分之活性碳,例如添加有氧化銅及氧化鋅之活性碳。添加有金屬之活性碳於活性碳表面附著有金屬或其化合物,金屬相對於活性碳之濃度以金屬換算計為1~10質量%左右。 第二處理部15係利用即便甲酸之濃度為低濃度亦能夠高速吸附之物理吸附而對甲酸進行處理,因此可將甲酸降低至0.5體積ppm以下。又,第一處理部13之出口氣體中之甲酸濃度降低至ppm等級,因此即便於第二處理部15中生成來自甲酸之一氧化碳,量亦非常少而不會產生特別問題。又,第二處理部15之多孔質吸附劑只要吸附少量之甲酸即可,可長時間維持吸附能力。 再者,關於第一處理部13中所使用之第一處理劑與第二處理部15中所使用之多孔質吸附劑之任一者,其形狀並無特別限定,粉末狀、粒狀、造粒而成之丸狀(pellet)均可。 又,甲酸處理裝置11係以乾式對包含甲酸蒸汽之氣體進行處理,燃燒除害或觸媒加熱除害中所需要之熱源並非必需,能夠節能,並且使裝置小型化。又,所使用之處理劑為一般使用之廉價之材料,不必使用高價之貴金屬系觸媒等,甲酸處理裝置11廉價,運轉成本亦廉價。 再者,第一處理部13與第二處理部15於圖1中於裝置內僅設有一個,但亦可分別設置複數個。於有複數個之情形時,可於複數個中同時流通氣體,於更換一部分之情形時亦於另一部分中流通氣體,藉此無需中斷處理。 甲酸使用裝置17只要為於某些處理中使用甲酸且於排氣中包含甲酸之裝置,則無特別限定,較佳為使用甲酸作為用以將焊料表面之氧化物還原之氣體之真空回流焊接裝置。作為真空回流焊接裝置中所使用之氣體,可使用由氮氣或氬氣、氖氣、氦氣等惰性氣體,或者氫氣或一氧化碳氣體等還原性氣體稀釋之甲酸。進而,氣體中除甲酸以外,亦可包含乙酸、丙酸、丁酸等羧酸,甲醇、乙醇等醇。 甲酸處理裝置11除甲酸使用裝置17之排氣以外,亦可用於自作為副產物等混入目標外生成之甲酸之氣體中去除甲酸,或者於以某種目的使用之氣體中混入甲酸之情形時自該氣體中去除甲酸。 [實施例] 以下,藉由參考例及實施例更詳細地說明本發明,但本發明並不由以下之實施例限定其範圍。 本發明者等人首先為了調查一般處理劑之甲酸吸附能力而進行了參考例1~11。 [參考例1~6] 於外徑1英吋之不鏽鋼管中以填充高度200 mm填充處理劑。向其中,使由氮氣稀釋之甲酸濃度為5體積%之處理氣體以1 L/min之速度流通。監測出口氣體之甲酸濃度,於超過5體積ppm之時點結束處理,測定處理開始至處理結束之處理時間,計算甲酸之處理量。將其結果示於表1。 沸石A:X型,陽離子=Ca,形狀=1.5 mmΦ,丸狀 吸濕沸石A:添加有25質量%之水分之沸石A 鹼石灰:氫氧化鈣79質量%、氫氧化鉀2質量%、氫氧化鈉質量1%,其他(如水分) 乾燥鹼石灰:乾燥上述之鹼石灰,使水分量為1質量%以下者 活性碳A:粒狀活性碳,破碎狀,粒徑=8~24目(2.36 mm~0.7 mm) 加入活性碳之鹼石灰:含有20質量%之粉末活性碳之鹼石灰,丸狀 [表1]
11‧‧‧甲酸處理裝置
13‧‧‧第一處理部
15‧‧‧第二處理部
17‧‧‧甲酸使用裝置11‧‧‧Formic acid treatment unit
13‧‧‧First Processing Department
15‧‧‧Second Processing Department
17‧‧‧ formic acid device
圖1係表示本發明之甲酸處理裝置1之圖。Fig. 1 is a view showing the formic acid processing apparatus 1 of the present invention.
11‧‧‧甲酸處理裝置 11‧‧‧Formic acid treatment unit
13‧‧‧第一處理部 13‧‧‧First Processing Department
15‧‧‧第二處理部 15‧‧‧Second Processing Department
17‧‧‧甲酸使用裝置 17‧‧‧ formic acid device
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