201223870 六、發明說明： 【發明所屬之技術領域】 本發明係關於一種對粗氨進行純化之氨純化系統。 【先前技術】 於半導體製造步驟及液晶製造步射，利用高純度之氨 作為用於說化物被膜之製作等之處理劑。此種高純度之氨 係藉由對粗氨進行純化以除去雜質而獲得。 粗氨中含有甲烷、乙烷、丙烷等低碳烴，具有更多碳數 之高碳烴，水分’以及氮、氧、氬等低彿點氣體作為雜 質。通常能獲得之粗氨之純度為99.5重量％左右。 根據半導體製造步驟及液晶製造步驟中之使用氨之步驟 之種類不同，4中之雜質之影響方式不同，但作為氨之純 度，要求為99.9999重量％以上，更佳為99 99999重量％以 上0 作為除去粗氨中含有之雜質之方法，已知有使用石夕膠、 合成沸s、活性碳等吸附劑吸附除去雜質之方法；蒸餾除 去雜質之方法。 例如，於日本專利特開2006_2〇641〇號公報中揭示有一 種氨純化系統，其包含：自.液體狀之粗氨中除去高沸點雜 質之第i蒸傑塔、將自蒸館塔導出之氣體狀之氨中含有 之雜質吸附除去之吸附塔、及由自吸附塔導出之氣體狀之 氨中除去低沸點雜質之第2蒸餾塔…於曰本專利特開 2003-183021唬公報中揭示有一種藉由將氣體狀之粗氨中 含有之水分利用包含氧化鋇之吸附劑吸附除去後進行蒸鶴 157804.doc 201223870 而對氨進行純化之方法。 於日本專利特開2006-20641 0號公報及日本專利特開 2003-183G21號公報中揭示之對氨進行純化之技術中在 將粗氧中含有之雜質吸附除去時，需要用於使氨自液體向 氣體進行相變之能量，在蒸館除去雜質時，需要用於使氨 在液體與氣體之間發生相變之能量。χ，自蒸料導出之 純化後之氣體狀之|冷凝而作為液體氨回收，因此於該冷 凝時亦需要能量1，於日本專利特開㈣641〇號公 報及日本專利特開2()()3_183()21號公報中揭示之對氨進行 純化之技術中，在將㈣中含有之雜質吸附、蒸顧除去、 進而冷凝而得到純化之液體氨為止之過程中，要消耗大旦 之能量。 里 【發明内容】 因此’本發明之目的在讀供__種可抑制能量之消 有效率地純化粗氨之氨純化系統。 本發明為-種氨純化系統，其係對含有雜質之粗氨進 純化者，其特徵在於包含： 7 貯留部’其貯留粗氨； 吸附部’其將自上述貯留部導出之粗氨中含有之 由吸附劑吸附除去； 貝错 ^ “’、飽。卩，其將沸點較氨低之低沸點雜質蒸餾除去. 第2蒸顧部，其將沸點較氨高之高沸點雜質蒸鶴除去. 冷凝部其將氨冷凝而作為液體氨回收； 分析部’其對自上述吸附部導出之氨中含有之雜質之濃 157804.doc 201223870 度進行分析； 配管，其形成自上述吸附部導出之氨流過之流路； 流路開關部’其開放或關閉上述配管+之流路；及 流路開關控制部，其基於上述分析部之分析結果而對開 放或關閉下述第丄〜第6閥門之流路之開關動作進行控制； 其中’上述配管包含： 第1配管，其連接在上述吸附部與上述第i蒸館部之間； 第2配管，其連接在上述第i蒸館部與上述第2蒸顧部之 間； 第3配管，其連接在上述第2蒸潑部與上述冷凝部之間，· 第4配管，其自上述第！配管分支並與上述第2配管連 接；及 第5配管，其於上述第2配管之較連接上述第依管之連 接部更為氨之流過方向下游侧自上述第2配管分支並與上 述第3配管連接； 上述流路開關部包含： 第1閥門，其設置於上述第1配管之較自上述第1配管分 支成上述第4配管之分支部更為氨之流過方向上游側； 第2閥門’其設置於上述p配管之較自上述第i配管分 支成上述第4配管之分支部更為氨之流過方向下游側； 第3閥門，其没置於上述第2配管之較自上述第2配管分 支成上述第5配管之分支部更為氨之流過方向下游側； 第4閥門’其設置於上述第3配管之較連接上述”配管 之連接部更為氨之流過方向上游側； 157804.doc 201223870 第5間門’其設置於上述第4配管；及 第6闕門，其設置於上述第5配管。 據本發明，氨純化系統包含貯留粗氨之貯留部、吸附 第1热餾部、第2蒸餾部、冷凝部、分析部、形成自吸 附P導出之氨流過之流路之配管、開放或關閉配管中之流 路之〃,L路開關部、及流路開關控制部。吸附部將自貯留部 導出之粗氨中含有之雜質吸附除去。第丨蒸餾部將沸點較 2低之低沸點雜質蒸餾除去。第2蒸餾部將沸點較氨高之 门弗』雜質蒸館除去。冷凝部將雜質除去後之氨冷凝而作 為^體氨回收。分析部對自吸附部導出之氨中含有之雜質 之濃度進行分析。崎包含··第1配管，其連接在吸附部 /、上述第1蒸餾部之間；第2配管，其連接在第丨蒸餾部與 第2蒸館部之間，·帛3配|，其連接在第❻德部與冷凝部 之間，第4配管，其自第丨配管分支並與第2配管連接；及 第配s，其於第2配管之較連接第4配管之連接部更為氨 之流過方向下游側自第2配管分支並與上述第3配管連接。 流路開關部包含：第1閥門，其設置於第i配管之較自第i 配官分支成第4配管之分支部更為氨之流過方向上游側； 第2閥門，其設置於第i配管之較自帛ι配管分支成第4配管 之刀支部更為氨之流過方向下游側；第3閥門，其設置於 第2配管之較自第2配管分支成第5配管之分支部更為氨之 流過方向下游側；第4閥門，其設置於第3配管之較連接第 5配官之連接部更為氨之流過方向上游側；第5閥門，其設 置於第4配管；及第6閥門，其設置於第5配管。 157804.doc 201223870 於以上述方式構成之氧純化系統中 貯留部導出之粗氨中含有之雜“ 先’吸附部將自 出之氨之H遙 ’、質吸附除去。自該吸附部導 之雜質之1=被導人至分㈣，藉由分㈣對氨中含有 流路開關控制部對設置於自吸附部導 资：=1 第1〜第6間門之開關動作進行控制 ^之 中’藉由分析部對自吸附部導 二之風純化系統 推广八 等出之氰中含有之雜質之濃度 ==根據該分析結果，可進行第咖部及第2蒸儲 讀除去之純化㈣，因此可省略不201223870 VI. Description of the Invention: [Technical Field of the Invention] The present invention relates to an ammonia purification system for purifying crude ammonia. [Prior Art] In the semiconductor manufacturing step and the liquid crystal production step, high-purity ammonia is used as a treatment agent for producing a compound film or the like. Such high purity ammonia is obtained by purifying crude ammonia to remove impurities. The crude ammonia contains low-carbon hydrocarbons such as methane, ethane, and propane, and has a higher carbon number of high-carbon hydrocarbons, and water and low-point gas such as nitrogen, oxygen, and argon as impurities. The purity of the crude ammonia which can usually be obtained is about 99.5 wt%. Depending on the type of semiconductor manufacturing step and the step of using ammonia in the liquid crystal manufacturing step, the influence of impurities in 4 is different, but the purity of ammonia is required to be 99.9999% by weight or more, more preferably 99 99999% by weight or more. A method of removing impurities contained in crude ammonia is known, and a method of adsorbing and removing impurities by using an adsorbent such as Shiqi gum, synthetic boiling s or activated carbon; and a method of removing impurities by distillation are known. An ammonia purification system comprising: an i-th steaming tower which removes high-boiling impurities from a liquid crude ammonia, and which is derived from a steaming tower, is disclosed in Japanese Laid-Open Patent Publication No. 2006-2〇641〇. An adsorption column for adsorbing and removing impurities contained in gaseous ammonia, and a second distillation column for removing low-boiling impurities from gaseous ammonia derived from the adsorption column are disclosed in Japanese Laid-Open Patent Publication No. 2003-183021. A method for purifying ammonia by adsorbing and removing water contained in gaseous crude ammonia by using an adsorbent containing cerium oxide, and then performing steaming 157804.doc 201223870. In the technique for purifying ammonia disclosed in Japanese Laid-Open Patent Publication No. 2006-20641 0 and Japanese Patent Laid-Open Publication No. 2003-183G21, when the impurities contained in the crude oxygen are adsorbed and removed, it is required to be used for the ammonia from the liquid. The energy of the phase change to the gas, when removing impurities from the vaporizer, requires energy for the phase change of ammonia between the liquid and the gas. χ 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化 纯化In the technique for purifying ammonia disclosed in Japanese Patent Publication No. 21-183, the energy contained in (4) is adsorbed, distilled, and condensed to obtain purified liquid ammonia, and energy of a large amount of energy is consumed. SUMMARY OF THE INVENTION Therefore, the object of the present invention is to improve the ammonia purification system for the purification of crude ammonia by suppressing the elimination of energy. The present invention is an ammonia purification system which is obtained by purifying crude ammonia containing impurities, and comprises: 7 a storage portion which stores crude ammonia; and an adsorption portion which contains the crude ammonia derived from the storage portion. It is adsorbed and removed by the adsorbent; Beibei ^ ", saturated. 卩, which removes low-boiling impurities with a lower boiling point than ammonia. The second steaming part, which removes high-boiling impurities with a higher boiling point than ammonia. The condensing unit condenses ammonia to recover as liquid ammonia; the analysis unit 'analyzes the concentration of impurities contained in the ammonia derived from the adsorption unit, 157804.doc 201223870 degrees; and the piping forms an ammonia stream derived from the adsorption unit a flow path; a flow path switch unit that opens or closes the flow path of the pipe +; and a flow path switch control unit that opens or closes the following third to sixth valves based on the analysis result of the analysis unit The switch operation of the flow path is controlled; wherein the pipe includes: a first pipe connected between the adsorption unit and the i-th steam column; and a second pipe connected to the i-th steam column and the first pipe 2 steaming department a third pipe connected between the second steaming portion and the condensation portion, a fourth pipe branched from the first pipe and connected to the second pipe, and a fifth pipe The second pipe is connected to the third pipe from the second pipe and connected to the third pipe, and the connecting portion of the second pipe is connected to the third pipe. The flow path switch unit includes: The first pipe is branched from the first pipe to the branch portion of the fourth pipe in the flow direction upstream of the ammonia flow, and the second valve is disposed in the p pipe from the i-th pipe. The branch portion of the fourth pipe is further flowed in the downstream direction of the ammonia flow; and the third valve is disposed in the branch portion of the second pipe which is not branched from the second pipe to the fifth pipe, and flows more ammonia. The fourth valve is disposed on the upstream side of the third pipe in which the connection portion of the pipe is connected to the above-mentioned "the pipe is more upstream." 157804.doc 201223870 The fifth door is disposed in the fourth pipe. And the sixth trick, which is set in the above 5 piping. According to the present invention, the ammonia purification system includes a storage portion for storing crude ammonia, a first hot distillation unit, a second distillation unit, a condensation unit, an analysis unit, and a pipe for forming a flow path through which ammonia derived from the adsorption P flows, or The flow path in the piping is closed, the L-channel switch unit, and the flow path switch control unit. The adsorption unit adsorbs and removes impurities contained in the crude ammonia derived from the storage portion. The second distillation section distills off low-boiling impurities having a boiling point lower than 2. The second distillation section removes the impurity of the Mentor's impurity boiling point higher than that of ammonia. The condensing portion condenses the ammonia after the impurities are removed and recovers as a body ammonia. The analysis unit analyzes the concentration of impurities contained in the ammonia derived from the adsorption unit. The first pipe includes a first pipe connected between the adsorption unit and the first distillation unit, and a second pipe connected between the second distillation unit and the second steaming unit, and a 帛3 matching| The fourth pipe is connected between the first pipe and the condensing portion, and the fourth pipe is branched from the second pipe and connected to the second pipe; and the second pipe is connected to the second pipe. The downstream side of the flow direction of ammonia flows from the second pipe and is connected to the third pipe. The flow path switch unit includes a first valve that is disposed on the upstream side of the flow path of the i-th pipe from the branch of the fourth pipe to the fourth pipe, and the second valve that is disposed at the i-th valve The knives of the fourth pipe are branched from the 配ι pipe to the downstream side of the ammonia flow direction, and the third valve is provided in the branch of the second pipe from the second pipe to the fifth pipe. The fourth valve is disposed on the upstream side of the third pipe with a connection portion connecting the fifth valve to the ammonia flow direction, and the fifth valve is disposed at the fourth pipe; And the sixth valve is provided in the fifth pipe. 157804.doc 201223870 In the oxygen purification system constructed as described above, the impurity contained in the crude ammonia derived from the storage portion of the oxygen storage system is removed, and the adsorption is removed from the adsorption portion. 1 = the person to be led to the minute (4), by means of the (4) control of the flow path switch control unit in the ammonia, the control operation of the self-adsorbing unit guide: =1, the first to the sixth door are controlled. By the analysis unit, the concentration of the impurities contained in the cyanide of the eight-equivalent is purified by the air purification system of the self-adsorption section. == According to the analysis result, the purification of the third portion and the second steam storage read and remove can be performed (four), Can be omitted
=純化動作。藉此，可抑制能量之消耗而有效率地純I 粗氣。 、 發月之氨純化系統中，較佳為上述流路開關控制 部進行下述之控制： ;上述刀析部之分析結果為顯示低沸點雜質之濃度未達 特定值且㈣_質之濃度未達特定值之分析結果的情形 夺使上述第1閥門、上述第5閥門及上述第6閥門開放， 使上述第2閥門、上述第3閥門及上述第*閥門關閉； ；述刀析。卩之分析結果為顯示低沸點雜質之濃度為特 定值以上且^弗點雜質之濃度未達特定值之分析結果的情 开/ k使上述第1閥門、上述第2閥門及上述第6閥門開 放使上述第3閥門、上述第4閥門及上述第5閥門關閉； 於上述分析部之分析結果為顯示低沸點雜質之濃度未達 特定值且兩彿點雜質之濃度為特定值以上之分析結果的情 形時，使上述第丨閥門、上述第5閥門、上述第3閥門及上 157804.doc 201223870 述第4閥門開放，使上述第2閥門及上述第6閥門關閉，· 於上述分析部之分析結果為顯示低沸點雜質之濃度為特 疋值以上且南沸點雜質之濃度為特定值以上之分析結果的 情形時，使上述第1閥門、上述第2閥門、上述第3閥門及 上述第4閥門開放，使上述第5閥門及上述第6閥門關閉。 根據本發明，流路開關控制部基於分析部之分析結果， 進行以下四種模式之控制。於第丨模式中，在分析部之分 析結果為顯示低沸點雜質之濃度未達特定值且高沸點雜質 之濃度未達特定值之分析結果的情形時，流路開關控制部 進行下述之控制：使第1閥門、第5閥門及第6閥門開放， 使第2閥門、第3閥門及第4閥門關閉。藉此，氨純化系統 對於自吸附部導出之氨，不進行第丨蒸餾部及第2蒸餾部中 之蒸餾除去之純化動作，使自吸附部導出之氨流過第丄配 管、第4配管、第2配管、第5配管及第3配管而導入至冷凝 部，從而可作為液體氨進行回收。 又，於第2模式中，在分析部之分析結果為顯示低沸點 雜質之濃度為特定值以上且高沸點雜質之濃度未達特定值 之分析結果的情形時，流路開關控制部進行下述之控制： 使第1閥門、第2閥門及第6閥門開放，使第3閥門、第4閥 門及第5閥門關閉。藉此，氨純化系統對於自吸附部導出 之氨’進行第1蒸餾部中之蒸餾除去之純化動作，不進行 第2蒸德部中之蒸餾除去之純化動作，使自吸附部導出之 氨流過第1配管、第2配管、第5配管及第3配管而導入至冷 凝部，從而可作為液體氨進行回收。 157804.doc -10· 201223870 又’於第3模式中，在分析部之分析結果為顯示低沸點 雜質之濃度未達特定值且高沸點雜質之濃度為狀值以上 之分析結果的情形時，流路開關控制部進行下述之控制： 使第1閥門、第5閥門、第3閥門及第4閥門開放，使第2閥 門及第6閥門關閉。藉& ’氨純化系統對於自吸附部導出 之氨，進行第2蒸餾部中之蒸餾除去之純化動作，不進行 第1蒸餾部中之蒸餾除去之純化動作，使自吸附部導出之 氨流過第1配管、第4配管、第2配管及第3配管而導入至冷 凝部’從而可作為液體氨進行回收。 又，於第4模式中，在分析部之分析結果為顯示低沸點 雜質之濃度為特定值以上且高沸點雜質之濃度為特定值以 上之分析結果的情形時，流路開關控制部進行下述之控 制：使第1閥門、第2閥門、第3閥門及第4閥門開放，使第 5閥門及第6閥門關閉。藉此，氨純化系統對於自吸附部導 出之氨，進行第1蒸餾部及第2蒸餾部中之蒸餾除去之純化 動作’使自吸附部導出之氨流過第1配管、第2配管及第3 配管而導入至冷凝部，從而可作為液體氨進行回收。 又，本發明之氨純化系統中，較佳為上述配管包含第6 配管’該第6配管連接在上述吸附部與上述貯留部之間， 开〆成直至上述分析部之分析結束為止自上述吸附部導出之 氨朝向上述貯留部流過之流路。 根據本發明，形成自上述吸附部導出之氨流過之流路之 配管包含第6配管，該第6配管連接在吸附部與貯留部之 間’形成直至分析部之分析結束為止自吸附部導出之氨朝 157804.doc -11 - 201223870 向貯留部流過之流路。藉此，直至分析部之分析結束為止 之期間’可使自吸附部導出之氨經由第6配管返回至貯留 部。 又，本發明之氣純化系統中，較佳為上述吸附部包含將 粗氨中含有之雜質藉由吸附劑吸附除去之複數個吸附部； 上述複數個吸附部以彼此相區別之狀態被導入自上述貯 留部導出之粗氨。 根據本發明，吸附部包含將粗氨中含有之雜質藉由吸附 劑吸附除去之複數個吸附部，且該複數個吸附部以彼此相 區別之狀態被導入自貯留部導出之粗氨。藉此，於利用一 個吸附部將粗氨中含有之雜質吸附除去之期間，可對使用 完之其他吸附部進行再生處理以便可利用使用完之其他吸 附部再次進行吸附除去動作。 又’本發明之錢化系統中，較佳為上述分析部包含氣 相層析裝置及腔體震盪吸收光譜分析裝置； 對於自上述吸附部導出之氨，湘氣相層析裝置分析甲 院濃度’利用腔體震盪吸收光譜分析裝置分析水分濃度。 據本發明，分析部包含氣相層析裂置及腔體震盈吸收 ^普分析裝置。而且，對於自吸附部導出之氨，利用氣相 :析裝置分析甲烷漢度，利用腔體震盪吸收光譜分析裝置 刀析水刀/農度。藉此’流路開關控制部可基於以由氣相層 析裝置分析之作為低彿點雜質之甲烧之濃度、及由腔體震 盧吸收光譜分析裝置分析之作為高濟點雜質之水分之濃度 所不的分析結果，控制第1〜第6閥門之開關動作。 157804.doc 201223870 又’本發明之氨純化系統中，較佳為上述吸附劑為選自 合成彿石'活性碳中之至少一種無機多孔質吸附劑。 根據本發明，吸附部中所使用之吸附劑為選自合成沸 石、活性碳中之至少一種無機多孔質吸附劑。藉由使用合 成彿石作為吸附劑’能夠效率良好地吸附除去粗氨中含有 之水分，藉由使用活性碳作為吸附劑，能夠效率良好地吸 附除去粗氨中含有之烴系之雜質。 本發明之目的、特色及優點藉由下述詳細之說明及圖式 變得更加明確。 【實施方式】 以下，參考圖式對本發明之較佳實施形態進行詳細說 日月。 '' 圖1係表示本發明之一實施形態之氨純化系統2 〇 〇之構成 之圖。圖2係表示氨純化系統200之構成之方塊圖。 本實施形態之氨純化系統200為對含有雜質之粗氨進行 純化之系、統。粗氨中包含甲烷、乙烷、丙烷等低碳烴，具 有更多碳數之高碳烴，水分，以及氮、氧、氬等低沸點氣 體作為雜質。即’減中包含滞點較氨⑽點為_33 44。〇 低之低碳烴、低沸點氣體等低彿點雜質、以及沸點較氨高 之高碳煙、水分等高沸點雜質。 、氨純化系統200包含作為貯留部之貯留罐i、吸附部2、 /刀析部3、作為第！蒸顧部之第i蒸潑塔4、作為第2蒸館部 :第勒塔5、作為冷凝部之冷凝器6、形成自吸附部2導 之風流過之流路之配管8、開放或關閉配管8中之流路之 157804.doc 13 201223870 流路開關部9、以及控制部10而構成。 貝丁留罐1為貯留粗氨者。貯留罐1只要為具有耐壓性及财 腐蝕性之保溫容器’則並無特別限制。該貯留罐"宁留作 為液體氨之粗氨，且藉由控制部1G之卫作條件控制部1〇2 控制為溫度及壓力達到一定條件。於貯留罐丨之上部，在 貯留液體氨之狀態下形成有氣相。於將粗氨自貯留罐1導 及附邛2時，可作為液體氨而導出，但本實施形態 中，將粗氨自上述氣相中作為氣體狀之氨而導出。於貯留 罐1與吸附部2之間連接有供給配管11，自貯留罐丨導出之 沣氨机過t、給配管丨丨而供給至吸附部2之第1吸附塔21或者 第2吸附塔22。再者，於粗氨向第1吸附塔21或者第2吸附 =22供、”。時，藉由設置於供給配管11之供給用閥門12、13 進行流路之開關動作。 吸附部2將自貯留罐丨導出之氣體狀之粗氨令含有之雜質 藉由吸附劑吸附除去。本實施形態中，吸附部2包含第^吸 附塔21與第2吸附塔22。第〗吸附塔21與第2吸附塔22為相 同構成，且以彼此相區別之狀態被導入自貯留罐丨導出之 氣體狀之粗氨。藉此，於例如利用第丨吸附塔2丨將粗氨中 含有之雜質吸附除去之期間，可對使用完之第2吸附塔Μ 進订再生處理以便可利用使用完之第2吸附塔22再次進行 吸附除去動作。 作為填充於第1吸附塔2 1及第2吸附塔22中之吸附劑，可 列舉出合成沸石、活性碳等無機多孔質吸附劑。作為合成 沸石，可列舉出微孔徑不同之MS_3A(微孔徑為3 A)、Ms_ 157804.doc •14. 201223870 4八（微孔徑為4人）、厘8-5入（微孔徑為5人）、]^8-13：^(微孔 徑為9人）。本實施形態中，作為吸附劑，使用烴及水分之 吸附能力優異之MS-13X、水分之吸附能力優異之MS-3A、烴之吸附能力優異之（MS-4A+MS-5A)層疊而成者。 於該層疊之吸附劑中混合比為MS-13X : MS-3A : (MS-4A+MS-5A)=1:1:1。 又’第1吸附塔21及第2吸附塔22藉由控制部10之工作條 件控制部102而控制溫度及壓力。具體而言，第1吸附塔21 及第2吸附塔22中之溫度被控制為〇〜60。(：，壓力被控制為 0.1〜1.0 MPa。於第1吸附塔21及第2吸附塔22之溫度未達 〇°C時’需要進行將吸附除去雜質時產生之吸附熱加以除 去之冷卻，從而有能量效率降低之虞。於第1吸附塔21及 第2吸附塔22之溫度超過601時，有吸附劑對雜質之吸附 能力降低之虞。又，於第1吸附塔21及第2吸附塔22之壓力 未達0.1 MPa時，有吸附劑對雜質之吸附能力降低之虞。 於第1吸附塔21及第2吸附塔22之壓力超過1.0 MPa時，為 維持在一定壓力下，需要大量之能量，從而有能量效率降 低之虞。 又，關於第1吸附塔21及第2吸附塔22中之線速度（Iinear velocity) ’每單位時間内將粗氨供給至第丨吸附塔2丨或第2 及附塔 22 之罝換算成 NTP(normal temperature and pressure ’常溫常壓）下之氣體體積並除以第1吸附塔2丨或 第2吸附塔22之空塔截面積而求出之值的範圍較佳為 0.1〜5.0 m/秒。於線速度未達〇. 1 m/秒時，吸附除去雜質需 157804.doc •15· 201223870 要長時間’因此不佳，於線速度超過5.0 m/秒時，吸附除 去雜質時產生之吸附熱之除去未充分進行，從而有吸附劑 對雜質之吸附能力降低之虞。 分析部3對自吸附部2導出之氣體狀之氨中含有之雜質之 濃度進行。本實施形態中析部3包含氣相層析裝 置（GC-PDD :脈衝放電型檢測器）31與腔體震盪吸收光譜 分析裝置（CRDS)32。作為氣相層析裝置31，例如可列舉出 GC-4000(GL Sciences股份有限公司製）$為腔體震盪吸 收光4分析裝置32，例如可列舉出MT〇_Lp七 Optics公司製）。 々本實施形態巾，對於自吸附部2導出氣體狀之氨，利用 孔相層析裝置31分析甲貌濃度，利腔體震盈吸收光譜分 析裝置32分析水分濃度。藉此，後述流路開關控制部⑻ 可基於以由氣相層析裝置31分析之作為低沸點雜質之子炫 及由腔體震I吸收光譜分析裝置32分析之作為高 9之開關二分之濃度所示的分析結果’控制流路開關部 第1蒸餾塔4將自吸附部2導 ^ ^ 等出之轧體狀之虱中含有之涛 點車乂乳低之低沸點雜質蒸 ^ ^ 壓力等工作條件藉由控 又 ^ 〇 制。卩10之工作條件控制部102而控 Z幻相塔4係自下依序形成 餾部44、中央空間部们、 下。P条 上°卩洛饀部4 2、上部空間邱4彳 於底部空間部45設置有 Π°Μ1， ^ Α 5,. 再/弗器45a，於上部空間部41設置 有冷凝器41a。真池哭/ic, 直 ° a自外部供給有例如加熱水等加 157804.doc •16- 201223870 試樣之再沸’冷凝器41a中自外部供給有例 如7卩水4冷卻介質以支持試樣之冷凝。 ::至第i蒸飽塔4之中央空間部43之氣體狀之氨於上部 :。部42中上升’與流下之回流液進行氣液接觸而被精 1 ’上升之氣相中含有之氨於回流液中溶解液化，沸 點較溶解於回流液中之氨低之低滿點雜質被氣化。此時， 低'弗點雜質被除去而被冷凝純化之氨流下至底部空間部4 $ 後’除向上部蒸顧部42之上部回流之一部分以外，均自底 部空間部45導出。另一方面，低沸點雜質上升至上部空間 部41而成為濃縮氣體，藉由冷凝器4u進行冷卻處理而連 續地作為廢氣排出。 第2蒸餾塔5將自吸附部2或第1蒸餾塔4導出之氨中含有 之沸點較氨高之高沸點雜質蒸館除去。第2蒸儲塔5中之溫 度、壓力等工作條件藉由控制部1〇之工作條件控制部102 而控制。第2蒸顧塔5具有與第！蒸麵塔4同樣之構造，形成 有底。P工間部55、下部蒸餾部54、中央空間部53、上部蒸 餾。卩52上部空間部51，於底部空間部55設置有再沸器 55a，於上部空間部51設置有冷凝器5ia〇 導入至第2蒸館塔5之中央空間部53之氨一邊與於下部蒸 餾。卩54中上升之氨氣進行氣液接觸，一邊移動至底部空間 55於是’被再彿而氣化之氨氣一邊與流下之溶液進行 氣液接觸，一邊經由下部蒸餾部54、中央空間部53及上部 蒸館部52進行純化。此時，蒸館純化之氨氣到達上部空間 4 51後，藉由冷凝器5U進行冷卻處理而自上部空間部μ 157804.doc 201223870 導出。另一方面’高沸點雜質流下至底部空間部55而成為 濃縮液’自底部空間部55作為廢液而排出。 冷凝器6將純化後之氨冷凝而作為液體氨回收，回收之 液體氨貯留於回收罐61中。冷凝器6中之溫度等工作條件 藉由控制部10之工作條件控制部102而控制。 又，本實施形態之氨純化系統200包含形成自吸附部2導 出之氨流過之流路之配管8。該配管8包含：第1配管8 1、 第2配管82、第3配管83、第4配管84、第5配管85、第6配 管86及第7配管87。第1配管81連接在吸附部2與第1蒸餾塔 4之間。第2配管82連接在第1蒸餾塔4與第2蒸餾塔5之間。 第3配管83連接在第2蒸餾塔5與冷凝器6之間。第4配管84 自第1配管81分支並與第2配管82連接。第5配管85於第2配 官82之較連接第4配管84之連接部更為氨之流過方向下游 側自第2配管82分支並與第3配管83連接。第6配管86連接 在吸附部2與貯留罐1之間，形成直至分析部3之分析結束 為止自吸附部2導出之氨朝向貯留罐〗流過之流路。直至利 用氣相層析裝置31進行之分析結束為止需要1〇分鐘左右之 時間，直至利用腔體震盪吸收光譜分析裝置32進行之分析 結束為止需要20〜30分鐘左右之時間。於直至分析部3之分 析結束為止之期間，藉由第6配管8 6可將自吸附部2導出之 氨經由第6配管86返回至貯留罐！。第7配管87自第i配管8ι 分支並與分析部3連接，形成自吸附部2導出之氨之一部分 朝向分析部3流過之流路。 又，本實施形態之氨純化系統2〇〇包含開放或關閉配管8 157804.doc -18 · 201223870 中之流路之流路開關部9。該流路開關部9包含第丨閥門 91、第2閥門92、第3閥門93、第4閥門94、第5閥門95、第 6閥門96、第7閥門97及第8閥門98。第1閥門91設置於第】 配管81之較自第1配管81分支成第4配管84之分支部更為氨 之流過方向上游側。第2閥門92設置於第i配管81之較自第 1配管81分支成第4配管84之分支部更為氨之流過方向下游 側。第3閥門93設置於第2配管82之較自第2配管82分支成 第5配管85之分支部更為氨之流過方向下游側。第4閥門％ 設置於第3配管83之較連接第5配管85之連接部更為氨之流 過方向上游側。第5閥門9S設置於第4配管Μ。第6閥門96 設置於第5配管85。第7閥門97設置於第6配管86。第8閥門 98設置於第7配管87。 以上述；$式構成之本貫施形態之氨純化系統2〇〇中，首 先，吸附部2將自貯留罐1導出之粗氨中含有之雜質吸附除 去。此.時，控制部10之流路開關控制部101進行下述之控 制：使第1閥門91、第2閥門92、第3閥門93、第4閥門94、 第5閥門95及第6閥門96關閉，使第7閥門97及第8閥門98開 放。藉此，自吸附部2導出之氨之一部分（分析部3之分析 所需之極少量之氨）流過第7配管87而導入至分析部3，藉 由分析部3對氨中含有之雜質之濃度進行分析。又，自吸 附部2導出之氨中除導入至分析部3之極少量之氨以外之殘 餘之氨直至分析部3之分析結束為止之期間，流過第6配管 86返回至貯留罐1。 而且，本實施形態之氨純化系統200中，控制部1〇之流 157804.doc -19· 201223870 路開關控制部ΠΠ基於分析部3之分析結果，對開放或關閉 流路開關部9中之配管8之流路之開關動作進行控制。氨純 化系統2〇〇中，藉由分析部3對自吸附部2導出之氨中含有 之雜質之濃度進行分析，根據該分析結果，可進行第1蒸 餾塔4及第2蒸餾塔5中之蒸餾除去之純化動作，因此可省 略不需要之蒸餾除去之純化動作，藉此可抑制能量之消耗 而有效率地純化粗氨β 其次，對本實施形態之氨純化系統2〇〇中之更具體之純 化動作進行說明。本實施形態之氨純化系統2〇〇中，流路 開關控制部101基於分析部3之分析結果，進行以下四種模 式之控制。 <第1模式> 圖3係表示於分析部3之分析結果為低沸點雜質及高沸點 雜質之濃度未達特定值之情形時配管8内之氨之流過狀態 之圖。於第1模式中，在分析部3之分析結果為顯示低沸點 雜質之濃度未達特定值（例如，甲烷之濃度未達3〇 ppb)且 尚沸點雜質之濃度未達特定值（例如，水分之濃度未達3〇 ppb)的分析結果時’流路開關控制部1〇1進行下述之控 制··使第1閥門91、第5閥門95及第6閥門96開放，使第2閥 門92、第3閥門93、第4閥門94及第7閥門97關閉。再者， 流路開關控制部101對於第8閥門98進行使之一直開放之控 制，該第8閥門98設置於自第1配管8丨分支並與分析部3連 接且分析部3之分析所需之極少量之氨流過的第7配管87。 如上所述’基於分析部3之分析結果而控制流路開關部9 157804.doc -20- 201223870 一 開關動作之氛純化系統200對於自吸附部2導出 之氨，不進行第i蒸館部4及第2蒸顧部5甲之蒸館除去之純 化動作，使自吸附部2導出之氨流過第1配管81、第4配管 84、第2配管82、第5配管85及第3配管83而導入至冷凝器 6,從而可作為液體氨進行回收。 <第2模式> 圖4係表示於分析部3之分析結果為低沸點雜質之濃度為 特定值以上且高㈣雜質之濃度未達特定值之情形時配管 8内之氨之流過狀態之圖。於第2模式中，在分析部3之分 析結果為顯示低沸點雜質之濃度為特定值（例如，甲烷之 濃度為30 ppb)以上且高濟點雜質之濃度未達特定值（例 如’水分之濃度未達30 ppb)的分析結果時，流路開關控制 部HH進行下述之控制：使第！閥門91、第2閥門％及第6閥 門96開放，使第3閥門93、第4閥門94、第5閥門％及第項 門97關閉。再者，流路開關控制部1〇1對於第8間門％進行 使之一直開放之控制，該第8閥門98設置於自第！配管。分 支並與分析部3連接且分析部3之分析所需之極少量之氨流 過的第7配管87。 如上所述，基於分析部3之分析結果而控制流路開關部9 之各閥門之開關動作之氨純化系統2〇〇對於自吸附部2導出 之氨，進行第1蒸餾部4中之蒸餾除去之純化動作，不進行 第2蒸顧塔5中之蒸館除去之純化動作，使自吸附部2導出 之氨流過第1配管81、第2配管82、第5配管85及第3配管们 而導入至冷凝器6’從而可作為液體氨進行回收。 J57804.doc •21 · 201223870 〈第3模式> 圖5係表示於分析部3之分析結果為低沸點雜質之濃度未 達特定值且高沸點雜質之濃度為特定值以上之情形時配管 8内之氨之流過狀態之圖。於第3模式中，在分析部3之分 析結果為顯示低沸點雜質之濃度未達特定值（例如，甲烷 之濃度未達30 ppb)且高沸點雜質之濃度為特定值（例如， 水分之濃度為30 ppb)以上的分析結果時，流路開關控制部 1〇1進行下述之控制：使第i閥門91、第5閥門95、第3閥門 93及第4閥門94開放，使第2閥門92、第6閥門96及第7閥門 97關閉。再者，流路開關控制部1〇1對於第8閥門％進行使 之一直開放之控制，該第8閥門98設置於自第i配管81分支 並與分析部3連接且分析部3之分析所需之極少量之氨流過 的第7配管87。 如上所述，基於分析部3之分析結果而控制流路開關部9 之各閥門之開關動作之氨純化系統2〇〇對於自吸附部2導出 之氨，進行第2蒸餾部5中之蒸餾除去之純化動作，不進行 第1蒸德塔4中之蒸館除去之純化動作，使自吸附部2導出 之氨流過第1配管81、第4配管M、第2配管82及第3配管μ 而導入至冷凝器6,從而可作為液體氨進行回收。 <第4模式> 圖6係表不於分析部3之分析結果為低沸點雜質及高沸點 雜質之濃度為特定值以上之情形時配管8内之氨之流過狀 態之圖。於第4模式中，在分析部3之分析結果為顯示低滞 點雜質之濃度為特定值(例如，曱烷之濃度為儿_以上 I57804.doc •22· 201223870 且高沸點雜質之濃度為特定值（例如，水分之濃度為30 ppb)以上的分析結果時，流路開關控制部1〇1進行下述之 控制：使第1閥門91、第2閥門92、第3閥門93及第4閥門94 開放’使第5閥門95、第6閥門96及第7閥門97關閉。再 者，流路開關控制部1〇1對於第8閥門98進行使之一直開放 之控制’該第8閥門98設置於自第1配管81分支並與分析部 3連接且分析部3之分析所需之極少量之氨流過的第7配管 87 〇 如上所述基於分析部3之分析結果而控制流路開關部9 之各閥門之開關動作之氨純化系統2〇〇對於自吸附部2導出 之氨，進行第1蒸館塔4及第2蒸館塔5中之蒸顧除去之純化 動作，使自吸附部2導出之氨流過第1配管81、第2配管82 及第3配管83而導入至冷凝器6，從而可作為液體氨進行回 收0 本發明於不脫離其精神或主要特徵之情況下能夠以其他 各種形態加以實施。因[上述實施形態於各個方面僅為 例示’本發明之範圍為申請專利範圍中所示者，並不受說 明書正文之任何約束。進而，屬於申請專利範圍之變形或 變全部為本發明之範圍内者。 【圖式簡單說明】 圖 圖1係表示本發明 之 實施形態之氨純化系統之構成 之 圖2係表示氨純化系統之構成之方塊圖。 圖3係表示於分析部之分士 析，，、。果為低沸點雜質及高沸 157804.doc -23- 201223870 雜質之濃度未達特定值之情形時配管内之氨之流過狀態之 圖。 圖4係表不於分析部之分析結果為低沸點雜質之濃度為 特定值以上且高彿點雜質之濃度未達特定值之情形時配管 内之氨之流過狀態之圖。 圖5係表示於分析部之分析結果為低沸點雜質之濃度未 達特定值且高沸點雜質之濃度為特^值以上之情形時配管 内之氨之流過狀態之圖。 圖6係表示於分析部之分析結果為低彿點雜質及高沸點 雜質之濃度為特定值以上之情形時配管内之氨之流過狀態 之圖。 【主要元件符號說明】 1 貯留罐 2 吸附部 3 分析部 4 第1蒸餾塔 5 第2蒸餾塔 6 冷凝器 7 分析時回收用冷凝器 8 配管 9 流路開閉部 10 控制部 11 供給配管 12 供給用閥門 157804.doc -24- 201223870 13 供給用閥門 21 第1吸附塔 22 第2吸附塔 31 氣相層析裝置 32 腔體震盪吸收光譜分析裝置 41 上部空間部 41a 冷凝器 42 上部蒸餾部 43 中央空間部 44 下部蒸餾部 45 底部空間部 45a 再沸器 51 上部空間部 51a 冷凝器 52 上部蒸餾部 53 中央空間部 54 下部蒸餾部 55 底部空間部 55a 再沸器 61 回收罐 81 第1配管 82 第2配管 83 第3配管 84 第4配管 157804.doc - 25 - 201223870 85 第5配管 86 第6配管 87 第7配管 91 第1閥門 92 第2閥門 93 第3閥門 94 第4閥門 95 第5閥門 96 第6閥門 97 第7閥門 98 第8閥門 101 流路開閉控制部 102 工作條件控制部 200 氨純化系統 157804.doc -26-= Purification action. Thereby, it is possible to suppress the consumption of energy and efficiently purify the crude gas. In the ammonia purification system of the moon, it is preferable that the flow path switch control unit performs the following control: the analysis result of the knife-removing portion is that the concentration of the low-boiling impurity is not up to a specific value and (4) the concentration of the substance is not When the analysis result of the specific value is reached, the first valve, the fifth valve, and the sixth valve are opened, and the second valve, the third valve, and the fourth valve are closed; The result of the analysis is that the first valve, the second valve, and the sixth valve are opened when the concentration of the low-boiling impurity is a specific value or more and the concentration of the impurity is not up to a specific value. The third valve, the fourth valve, and the fifth valve are closed. The analysis result of the analysis unit is an analysis result indicating that the concentration of the low-boiling impurities does not reach a specific value and the concentration of the two-point impurity is a specific value or more. In this case, the fourth valve, the fifth valve, the third valve, and the fourth valve of the above-mentioned 157804.doc 201223870 are opened, and the second valve and the sixth valve are closed, and the analysis result of the analysis unit is performed. When the concentration of the low-boiling impurities is not less than the characteristic value and the concentration of the south boiling point impurities is a specific value or more, the first valve, the second valve, the third valve, and the fourth valve are opened. The fifth valve and the sixth valve are closed. According to the invention, the flow path switch control unit performs the control of the following four modes based on the analysis result of the analysis unit. In the second mode, when the analysis result in the analysis section is that the concentration of the low-boiling impurities is not up to a specific value and the concentration of the high-boiling impurities is not up to a specific value, the flow path switch control section performs the following control. : The first valve, the fifth valve, and the sixth valve are opened, and the second valve, the third valve, and the fourth valve are closed. In the ammonia purification system, the ammonia derived from the adsorption unit is not subjected to the purification operation of the distillation in the second distillation section and the second distillation section, and the ammonia derived from the adsorption section flows through the second piping and the fourth piping. The second pipe, the fifth pipe, and the third pipe are introduced into the condensing portion, and can be recovered as liquid ammonia. In the second mode, when the analysis result of the analysis unit is that the concentration of the low-boiling impurities is a specific value or more and the concentration of the high-boiling impurities does not reach a specific value, the flow path switch control unit performs the following. Control: The first valve, the second valve, and the sixth valve are opened, and the third valve, the fourth valve, and the fifth valve are closed. In this way, the ammonia purification system performs the purification operation of distilling and removing the ammonia extracted from the adsorption unit in the first distillation section, and does not perform the purification operation of the distillation in the second vaporization section, thereby causing the ammonia flow derived from the adsorption section. The first pipe, the second pipe, the fifth pipe, and the third pipe are introduced into the condensation portion to be recovered as liquid ammonia. 157804.doc -10· 201223870 In the third mode, when the analysis result in the analysis unit is a case where the concentration of the low-boiling impurities is not up to a specific value and the concentration of the high-boiling impurities is a value or more, the flow is The switch control unit performs the following control: The first valve, the fifth valve, the third valve, and the fourth valve are opened to close the second valve and the sixth valve. In the ammonia purification system, the ammonia derived from the adsorption unit is subjected to a purification operation of distillation in the second distillation section, and the purification operation in the first distillation section is not performed, and the ammonia flow derived from the adsorption section is obtained. The first pipe, the fourth pipe, the second pipe, and the third pipe are introduced into the condensing unit', and can be recovered as liquid ammonia. In the fourth mode, when the analysis result of the analysis unit is that the concentration of the low-boiling impurities is a specific value or more and the concentration of the high-boiling impurities is a specific value or more, the flow path switch control unit performs the following. Control: The first valve, the second valve, the third valve, and the fourth valve are opened, and the fifth valve and the sixth valve are closed. In the ammonia purification system, the ammonia derived from the adsorption unit is subjected to a purification operation of distilling and removing the first distillation unit and the second distillation unit. The ammonia derived from the adsorption unit flows through the first pipe, the second pipe, and the first 3 The piping is introduced into the condensing section to be recovered as liquid ammonia. Further, in the ammonia purification system of the present invention, preferably, the pipe includes a sixth pipe, and the sixth pipe is connected between the adsorption unit and the storage unit, and is opened until the analysis of the analysis unit is completed. The ammonia derived from the portion is directed toward the flow path through which the storage portion flows. According to the present invention, the pipe forming the flow path through which the ammonia derived from the adsorption unit flows is included in the sixth pipe, and the sixth pipe is connected between the adsorption portion and the storage portion, and is formed from the adsorption portion until the analysis of the analysis portion is completed. The ammonia flows toward the storage section of 157804.doc -11 - 201223870. Thereby, the ammonia derived from the adsorption unit can be returned to the storage portion via the sixth pipe until the analysis of the analysis unit is completed. Further, in the gas purification system of the present invention, it is preferable that the adsorption unit includes a plurality of adsorption units that adsorb and remove impurities contained in the crude ammonia by the adsorbent; and the plurality of adsorption units are introduced from each other in a state different from each other. The crude ammonia derived from the storage portion. According to the invention, the adsorption unit includes a plurality of adsorption units for adsorbing and removing impurities contained in the crude ammonia by the adsorbent, and the plurality of adsorption units are introduced into the crude ammonia derived from the storage unit in a state of being distinguished from each other. Thereby, during the period in which the impurities contained in the crude ammonia are adsorbed and removed by one adsorption unit, the other adsorption portions that have been used can be regenerated so that the adsorption removal operation can be performed again by using the other adsorption portions that have been used. Further, in the money-making system of the present invention, preferably, the analysis unit includes a gas chromatograph device and a chamber oscillation absorption spectrum analyzer; and the ammonia derived from the adsorption unit is analyzed by a gas chromatography apparatus. 'Using a cavity oscillating absorption spectrometer to analyze the water concentration. According to the present invention, the analysis unit includes a gas chromatography to split and a chamber shock absorption analysis device. Further, for the ammonia derived from the adsorption section, the gas phase is analyzed by a gas phase analysis device, and the water knife/agricultural degree is analyzed by a cavity oscillation absorption spectrometer. Thereby, the flow path switch control unit can be based on the concentration of the smoldering gas which is analyzed as a low point impurity by the gas chromatograph device, and the moisture which is analyzed by the cavity shock absorption spectroscopy device as the high-point impurity. The analysis result of the concentration is not controlled, and the switching operation of the first to sixth valves is controlled. Further, in the ammonia purification system of the present invention, it is preferable that the adsorbent is at least one inorganic porous adsorbent selected from the group consisting of synthetic Fossil' activated carbon. According to the invention, the adsorbent used in the adsorption section is at least one inorganic porous adsorbent selected from the group consisting of synthetic zeolite and activated carbon. By using the synthetic fluorite as the adsorbent, the water contained in the crude ammonia can be efficiently adsorbed and removed, and by using activated carbon as the adsorbent, the hydrocarbon-based impurities contained in the crude ammonia can be efficiently adsorbed and removed. The objects, features, and advantages of the invention will be apparent from the description and drawings. [Embodiment] Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings. Fig. 1 is a view showing the configuration of an ammonia purification system 2 according to an embodiment of the present invention. 2 is a block diagram showing the construction of an ammonia purification system 200. The ammonia purification system 200 of the present embodiment is a system for purifying crude ammonia containing impurities. The crude ammonia contains low-carbon hydrocarbons such as methane, ethane, and propane, and has a higher carbon number of high-carbon hydrocarbons, water, and low-boiling gas such as nitrogen, oxygen, and argon as impurities. That is, the minus point contains a lag point that is _33 44 than the ammonia (10) point.低 Low-point hydrocarbons such as low-carbon hydrocarbons and low-boiling gases, and high-boiling impurities such as high-carbon fumes and moisture with a higher boiling point than ammonia. The ammonia purification system 200 includes a storage tank i as a storage portion, an adsorption unit 2, and a knife extraction unit 3 as a first! The i-th steaming tower 4 of the steaming portion, the second steaming column portion: the second column 5, the condenser 6 as the condensation portion, and the pipe 8 forming the flow path through which the air guided by the adsorption portion 2 flows, opening or closing The flow path 157804.doc 13 201223870 flow path switch unit 9 and the control unit 10 in the pipe 8 are configured. Bedding Retaining Tank 1 is for storing crude ammonia. The storage tank 1 is not particularly limited as long as it is a heat-resistant container having pressure resistance and corrosion resistance. The storage tank " is kept as a crude ammonia of liquid ammonia, and is controlled by the control condition control unit 1〇2 of the control unit 1G to reach a certain condition of temperature and pressure. On the upper part of the storage tank, a gas phase is formed in a state where liquid ammonia is stored. When crude ammonia is introduced from the storage tank 1 and the second layer, it can be derived as liquid ammonia. However, in the present embodiment, crude ammonia is derived as gaseous ammonia from the gas phase. A supply pipe 11 is connected between the storage tank 1 and the adsorption unit 2, and the ammonia pump that has been taken out from the storage tank 过 is supplied to the first adsorption tower 21 or the second adsorption tower 22 that is supplied to the adsorption unit 2 by the supply enthalpy. . In addition, when the crude ammonia is supplied to the first adsorption tower 21 or the second adsorption = 22, the flow switching operation is performed by the supply valves 12 and 13 provided in the supply pipe 11. The adsorption unit 2 will be self-contained. In the present embodiment, the adsorption unit 2 includes the second adsorption tower 21 and the second adsorption tower 22. The adsorption tower 21 and the second adsorption tower 21 are provided. The adsorption towers 22 have the same configuration, and are introduced into the gaseous crude ammonia derived from the storage tanks in a state different from each other. Thereby, the impurities contained in the crude ammonia are adsorbed and removed by, for example, the second adsorption tower 2丨. In the meantime, the used second adsorption tower can be subjected to a regeneration regeneration operation so that the second adsorption tower 22 can be used again to perform the adsorption removal operation. The first adsorption tower 2 1 and the second adsorption tower 22 are filled. Examples of the adsorbent include inorganic porous adsorbents such as synthetic zeolite and activated carbon. Examples of the synthetic zeolite include MS_3A (microporosity of 3 A) having a small pore diameter, and Ms_157804.doc • 14. 201223870 4:8 Aperture is 4 people), PCT is 8-5 (micro-aperture is 5) In the present embodiment, MS-13X which is excellent in adsorption ability of hydrocarbons and water, and MS-3A which is excellent in moisture adsorption capacity, and hydrocarbons are used as the adsorbent. The product with excellent adsorption capacity (MS-4A+MS-5A) is laminated. The mixing ratio of the adsorbent in the stack is MS-13X: MS-3A: (MS-4A+MS-5A)=1:1 Further, the first adsorption tower 21 and the second adsorption tower 22 control the temperature and pressure by the operating condition control unit 102 of the control unit 10. Specifically, the first adsorption tower 21 and the second adsorption tower 22 are The temperature is controlled to 〇~60. (: The pressure is controlled to 0.1 to 1.0 MPa. When the temperature of the first adsorption tower 21 and the second adsorption tower 22 is less than 〇 °C, it is required to carry out adsorption to remove impurities. The heat of adsorption is removed and the energy efficiency is lowered. When the temperature of the first adsorption tower 21 and the second adsorption tower 22 exceeds 601, the adsorption capacity of the adsorbent for impurities is lowered. When the pressure of the adsorption tower 21 and the second adsorption tower 22 is less than 0.1 MPa, the adsorption capacity of the adsorbent to impurities is lowered. The first adsorption tower 21 and the second adsorption tower 22 are When the pressure exceeds 1.0 MPa, a large amount of energy is required to maintain a certain pressure, which results in a decrease in energy efficiency. Further, the linear velocity (Iinear velocity) in each of the first adsorption tower 21 and the second adsorption tower 22 The crude ammonia is supplied to the second adsorption tower 2 or the second and the second column 22 per unit time, and is converted into a gas volume under NTP (normal temperature and pressure 'normal temperature and normal pressure) and divided by the first adsorption tower 2 or The range of the value obtained by the cross-sectional area of the second adsorption tower 22 is preferably 0.1 to 5.0 m/sec. When the line speed is less than 1 m/sec, the adsorption and removal of impurities requires 157804.doc •15· 201223870 to be long-term, so it is not good, when the linear velocity exceeds 5.0 m/s, the adsorption heat generated when adsorbing and removing impurities The removal is not sufficiently performed, so that the adsorption capacity of the adsorbent for impurities is lowered. The analysis unit 3 performs the concentration of the impurities contained in the gaseous ammonia derived from the adsorption unit 2. In the present embodiment, the analysis unit 3 includes a gas chromatograph (GC-PDD: pulse discharge type detector) 31 and a cavity oscillation absorption spectrum analyzer (CRDS) 32. For example, the GC-4000 (manufactured by GL Sciences Co., Ltd.) is a cavity oscillating absorbing light 4 analyzing device 32, and examples thereof include, for example, MT〇_Lp7 Optics Inc.). In the present embodiment, the gaseous ammonia is derived from the adsorption unit 2, the pore concentration is analyzed by the pore phase chromatography device 31, and the water concentration is analyzed by the positive chamber absorption absorption spectrum analyzer 32. Thereby, the flow path switch control unit (8), which will be described later, can be based on the concentration of the low-boiling impurity analyzed by the gas chromatograph device 31 and the concentration of the switch which is analyzed by the cavity shock I absorption spectrum analyzing device 32 as the high 9 switch. The analysis result shown in the 'control flow path switch unit's first distillation column 4 is a low-boiling point impurity steaming ^ ^ pressure which is contained in the rolled body shape which is obtained from the adsorption unit 2 Conditions are controlled by control. The operating condition control unit 102 of the crucible 10 controls the Z phantom phase tower 4 to sequentially form the distilling unit 44 and the central space unit. P 上 卩 卩 4 4 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2 2真池哭/ic, straight ° a from external supply such as heating water, etc. plus 157804.doc •16- 201223870 sample reboiler 'condenser 41a from the outside is supplied with, for example, 7 卩 water 4 cooling medium to support the sample Condensation. :: The gaseous ammonia to the central space portion 43 of the i-th steaming tower 4 is at the upper portion: The portion 42 rises in the gas-liquid contact with the reflux liquid flowing down, and the ammonia contained in the gas phase which is raised by the purification 1' is dissolved and liquefied in the reflux liquid, and the low-point impurity having a lower boiling point than the ammonia dissolved in the reflux liquid is gasification. At this time, the low-frozen impurity is removed, and the condensed and purified ammonia flows down to the bottom space portion 4$, and is discharged from the bottom space portion 45 except for a portion of the upper portion of the upper steaming portion 42. On the other hand, the low-boiling impurities rise to the upper space portion 41 and become a concentrated gas, and are cooled by the condenser 4u to be continuously discharged as exhaust gas. In the second distillation column 5, the high-boiling impurities having a higher boiling point than ammonia are contained in the ammonia derived from the adsorption unit 2 or the first distillation column 4, and are removed. The operating conditions such as temperature and pressure in the second steam storage tower 5 are controlled by the operating condition control unit 102 of the control unit 1 . The second steaming tower 5 has the same! The steaming tower 4 has the same structure and is formed with a bottom. The P intermediate portion 55, the lower distillation portion 54, the central space portion 53, and the upper portion are distilled. The upper space portion 51 of the crucible 52 is provided with a reboiler 55a in the bottom space portion 55, and the upper space portion 51 is provided with a condenser 5ia, which is introduced into the central space portion 53 of the second vaporization column 5, and is distilled in the lower portion. . The ammonia gas rising in the crucible 54 is brought into gas-liquid contact, and moves to the bottom space 55, and then the ammonia gas which is vaporized again is gas-liquid contacted with the solution flowing down, and passes through the lower distillation portion 54 and the central space portion 53. The upper steaming section 52 is purified. At this time, the ammonia gas purified by the steaming furnace reaches the upper space 4 51 and is cooled by the condenser 5U to be derived from the upper space portion μ 157804.doc 201223870. On the other hand, the "high-boiling impurities flow down to the bottom space portion 55 to become a concentrated liquid" is discharged from the bottom space portion 55 as a waste liquid. The condenser 6 condenses the purified ammonia to be recovered as liquid ammonia, and the recovered liquid ammonia is stored in the recovery tank 61. The operating conditions such as the temperature in the condenser 6 are controlled by the operating condition control unit 102 of the control unit 10. Further, the ammonia purification system 200 of the present embodiment includes a pipe 8 that forms a flow path through which the ammonia guided from the adsorption unit 2 flows. The pipe 8 includes a first pipe 8 1 , a second pipe 82 , a third pipe 83 , a fourth pipe 84 , a fifth pipe 85 , a sixth pipe 86 , and a seventh pipe 87 . The first pipe 81 is connected between the adsorption unit 2 and the first distillation column 4. The second pipe 82 is connected between the first distillation column 4 and the second distillation column 5. The third pipe 83 is connected between the second distillation column 5 and the condenser 6. The fourth pipe 84 branches from the first pipe 81 and is connected to the second pipe 82. The fifth pipe 85 is branched from the second pipe 82 and connected to the third pipe 83 at the connection portion of the second pipe 82 connected to the fourth pipe 84 to the downstream side in the flow direction of ammonia. The sixth pipe 86 is connected between the adsorption unit 2 and the storage tank 1 to form a flow path through which the ammonia derived from the adsorption unit 2 flows toward the storage tank until the analysis of the analysis unit 3 is completed. It takes about 1 minute until the analysis by the gas chromatography apparatus 31 is completed, and it takes about 20 to 30 minutes until the analysis by the cavity oscillation absorption spectrometer 32 is completed. During the period until the analysis of the analysis unit 3 is completed, the ammonia derived from the adsorption unit 2 can be returned to the storage tank via the sixth pipe 86 by the sixth pipe 86. . The seventh pipe 87 branches from the i-th pipe 8 1 and is connected to the analysis unit 3, and forms a flow path through which the ammonia portion derived from the adsorption unit 2 flows toward the analysis unit 3. Further, the ammonia purification system 2A of the present embodiment includes the flow path switch unit 9 that opens or closes the flow path in the pipe 8 157804.doc -18 · 201223870. The flow path switch unit 9 includes a second valve 91, a second valve 92, a third valve 93, a fourth valve 94, a fifth valve 95, a sixth valve 96, a seventh valve 97, and an eighth valve 98. The first valve 91 is provided on the upstream side in the flow direction of the ammonia branching portion 81 which is branched from the first pipe 81 into the fourth pipe 84. The second valve 92 is provided on the downstream side of the i-th pipe 81 which is branched from the first pipe 81 into the branch portion of the fourth pipe 84 in the flow direction of ammonia. The third valve 93 is provided on the downstream side of the second pipe 82 which is branched from the second pipe 82 into the branch portion of the fifth pipe 85 in the flow direction of ammonia. The fourth valve % is provided in the connection portion of the third pipe 83 to the fifth pipe 85 connected to the upstream side in the flow direction of ammonia. The fifth valve 9S is provided in the fourth pipe Μ. The sixth valve 96 is provided in the fifth pipe 85. The seventh valve 97 is provided in the sixth pipe 86. The eighth valve 98 is provided in the seventh pipe 87. In the ammonia purification system of the above-described embodiment of the present invention, the adsorption unit 2 first adsorbs and removes impurities contained in the crude ammonia derived from the storage tank 1. In this case, the flow path switch control unit 101 of the control unit 10 performs control such that the first valve 91, the second valve 92, the third valve 93, the fourth valve 94, the fifth valve 95, and the sixth valve 96 are provided. Closing, the seventh valve 97 and the eighth valve 98 are opened. Thereby, one part of the ammonia derived from the adsorption unit 2 (a very small amount of ammonia required for the analysis of the analysis unit 3) flows through the seventh pipe 87 and is introduced into the analysis unit 3, and the impurity contained in the ammonia is analyzed by the analysis unit 3. The concentration was analyzed. In addition, ammonia remaining in the ammonia derived from the absorbing portion 2 is returned to the storage tank 1 through the sixth pipe 86 until the analysis of the analysis unit 3 is completed until the analysis of the analysis unit 3 is completed. Further, in the ammonia purification system 200 of the present embodiment, the flow of the control unit 1 157804.doc -19·201223870 switch control unit 开放 opens or closes the piping in the flow path switch unit 9 based on the analysis result of the analysis unit 3 The switching action of the flow path of 8 is controlled. In the ammonia purification system, the concentration of the impurities contained in the ammonia derived from the adsorption unit 2 is analyzed by the analysis unit 3, and the first distillation column 4 and the second distillation column 5 can be performed based on the analysis results. Since the purification operation by distillation is omitted, the purification operation which is not required for distillation can be omitted, whereby the consumption of energy can be suppressed and the crude ammonia β can be efficiently purified. Next, the ammonia purification system of the present embodiment is more specifically The purification operation will be described. In the ammonia purification system 2 of the present embodiment, the flow path switch control unit 101 performs the following four modes of control based on the analysis result of the analysis unit 3. <First Mode> FIG. 3 is a view showing a flow state of ammonia in the pipe 8 when the analysis result of the analysis unit 3 is such that the concentration of the low-boiling impurities and the high-boiling impurities does not reach a specific value. In the first mode, the analysis result in the analysis section 3 is that the concentration of the low-boiling impurities is not up to a specific value (for example, the concentration of methane is less than 3 ppb) and the concentration of the boiling point impurities is not up to a specific value (for example, moisture). When the concentration is less than 3 ppb), the flow path switch control unit 1〇1 performs the following control. The first valve 91, the fifth valve 95, and the sixth valve 96 are opened, and the second valve 92 is opened. The third valve 93, the fourth valve 94, and the seventh valve 97 are closed. Further, the flow path switch control unit 101 controls the eighth valve 98 to be always open, and the eighth valve 98 is provided to be branched from the first pipe 8丨 and connected to the analysis unit 3, and the analysis unit 3 is required for analysis. The seventh pipe 87 through which a very small amount of ammonia flows. As described above, the flow channel switch unit 9 157804.doc -20-201223870 is controlled based on the analysis result of the analysis unit 3, and the atmosphere purification system 200 that is operated by the adsorption unit 2 does not perform the i-th vapor column unit 4 And the purification operation of the steaming chamber of the second steaming unit 5, the ammonia derived from the adsorption unit 2 flows through the first pipe 81, the fourth pipe 84, the second pipe 82, the fifth pipe 85, and the third pipe 83. It is introduced into the condenser 6, so that it can be recovered as liquid ammonia. <Second Mode> FIG. 4 shows a flow state of ammonia in the pipe 8 when the concentration of the low-boiling impurity is a specific value or more and the concentration of the high impurity does not reach a specific value in the analysis result of the analysis unit 3. Picture. In the second mode, the analysis result in the analysis unit 3 is that the concentration of the low-boiling impurities is a specific value (for example, the concentration of methane is 30 ppb) or more, and the concentration of the high-point impurity is not a specific value (for example, 'moisture When the concentration is less than 30 ppb), the flow path switch control unit HH performs the following control: The valve 91, the second valve %, and the sixth valve 96 are opened, and the third valve 93, the fourth valve 94, the fifth valve %, and the first door 97 are closed. Further, the flow path switch control unit 1〇1 controls the eighth door % to be kept open, and the eighth valve 98 is provided in the first! Piping. The seventh pipe 87 which is branched and connected to the analysis unit 3 and which has a very small amount of ammonia required for analysis of the analysis unit 3 flows. As described above, the ammonia purification system 2 that controls the switching operation of the valves of the flow path switch unit 9 based on the analysis result of the analysis unit 3 performs the distillation in the first distillation unit 4 on the ammonia derived from the adsorption unit 2. In the purification operation, the purification operation of the vapor removal in the second steaming tower 5 is not performed, and the ammonia derived from the adsorption unit 2 flows through the first pipe 81, the second pipe 82, the fifth pipe 85, and the third pipe. It is introduced into the condenser 6' so that it can be recovered as liquid ammonia. J57804.doc • 21 · 201223870 <3rd mode> Fig. 5 shows the case where the analysis result of the analysis unit 3 is such that the concentration of the low-boiling impurities does not reach a specific value and the concentration of the high-boiling impurities is a specific value or more. The flow of ammonia through the state. In the third mode, the analysis result in the analysis section 3 is that the concentration of the low-boiling impurities is not up to a specific value (for example, the concentration of methane is less than 30 ppb) and the concentration of the high-boiling impurities is a specific value (for example, the concentration of moisture) When the analysis result is 30 ppb or more, the flow path switch control unit 1〇1 performs control such that the i-th valve 91, the fifth valve 95, the third valve 93, and the fourth valve 94 are opened, and the second valve is opened. 92. The sixth valve 96 and the seventh valve 97 are closed. Further, the flow path switch control unit 1〇1 controls the eighth valve % to be always open, and the eighth valve 98 is provided in the analysis unit that is branched from the i-th pipe 81 and connected to the analysis unit 3 and analyzed by the analysis unit 3. The seventh pipe 87 through which a very small amount of ammonia flows is required. As described above, the ammonia purification system 2 that controls the switching operation of the valves of the flow path switch unit 9 based on the analysis result of the analysis unit 3 performs the distillation removal in the second distillation unit 5 on the ammonia derived from the adsorption unit 2. In the purification operation, the purification operation by the vapor removal in the first vaporization tower 4 is not performed, and the ammonia derived from the adsorption unit 2 flows through the first pipe 81, the fourth pipe M, the second pipe 82, and the third pipe μ. It is introduced into the condenser 6, so that it can be recovered as liquid ammonia. <Fourth Mode> Fig. 6 is a view showing a flow state of ammonia in the pipe 8 when the concentration of the low-boiling impurities and the high-boiling impurities is a specific value or more in the analysis result of the analysis unit 3. In the fourth mode, the analysis result in the analysis unit 3 is that the concentration of the low-stagnation impurity is a specific value (for example, the concentration of decane is __I57804.doc • 22·201223870 and the concentration of the high-boiling impurity is specific When the value of the analysis (for example, the concentration of water is 30 ppb) or more, the flow path switch control unit 1〇1 performs control such that the first valve 91, the second valve 92, the third valve 93, and the fourth valve are provided. 94 is opened to close the fifth valve 95, the sixth valve 96, and the seventh valve 97. Further, the flow path switch control unit 1〇1 controls the eighth valve 98 to be kept open. The eighth valve 98 is set. The seventh pipe 87 branched from the first pipe 81 and connected to the analysis unit 3 and having a very small amount of ammonia required for the analysis of the analysis unit 3 is controlled based on the analysis result of the analysis unit 3 as described above. The ammonia purification system of the switching operation of each of the valves of the first and second steaming towers 5, and the purification operation of the evaporation in the first steaming tower 4 and the second steaming tower 5, and the self-adsorption section 2 The derived ammonia flows through the first pipe 81, the second pipe 82, and the third pipe 83, and is introduced into the condenser 6. Therefore, it can be recovered as liquid ammonia. The present invention can be implemented in various other forms without departing from the spirit or main features thereof. [The above embodiments are merely illustrative in all respects. The present invention is not limited by the scope of the specification. Further, all modifications and variations of the scope of the invention are within the scope of the invention. [FIG. 1] FIG. 1 shows an embodiment of the present invention. Figure 2 of the structure of the ammonia purification system is a block diagram showing the structure of the ammonia purification system. Figure 3 shows the analysis of the analysis in the analysis section, and the results are low-boiling impurities and high boiling 157804.doc -23- 201223870 impurities A graph showing the flow state of ammonia in the pipe when the concentration is not at a specific value. Fig. 4 shows that the analysis result of the analysis portion is that the concentration of the low-boiling impurity is a specific value or more and the concentration of the impurity at the high point is not reached. A graph showing the flow state of ammonia in the piping in the case of a specific value. Fig. 5 shows that the analysis result in the analysis section is that the concentration of the low-boiling impurities is not up to a specific value and the high boiling point is mixed. FIG. 6 is a view showing a state in which the concentration of ammonia in the pipe is higher than the specific value. FIG. 6 is a case where the analysis result in the analysis unit is such that the concentration of the low-point impurity and the high-boiling impurity is a specific value or more. Diagram of the flow of ammonia in the piping. [Description of main components] 1 Storage tank 2 Adsorption unit 3 Analysis unit 4 First distillation column 5 Second distillation column 6 Condenser 7 Condensation recovery condenser 8 Pipe 9 flow Road opening and closing unit 10 Control unit 11 Supply pipe 12 Supply valve 157804.doc -24- 201223870 13 Supply valve 21 First adsorption tower 22 Second adsorption tower 31 Gas chromatography device 32 Cavity oscillation absorption spectrum analysis device 41 Upper portion Space portion 41a condenser 42 upper distillation portion 43 central space portion 44 lower distillation portion 45 bottom space portion 45a reboiler 51 upper space portion 51a condenser 52 upper distillation portion 53 central space portion 54 lower distillation portion 55 bottom space portion 55a Boiling tank 61 recovery tank 81 first piping 82 second piping 83 third piping 84 fourth piping 157804.doc - 25 - 201223870 85 fifth piping 86 sixth 87 7th pipe 91 1st valve 92 2nd valve 93 3rd valve 94 4th valve 95 5th valve 96 6th valve 97 7th valve 98 8th valve 101 Flow path opening and closing control unit 102 Operating condition control unit 200 Ammonia purification System 157804.doc -26-