TW201529484A - Method for treating a hydrofluoric acid-containing waste liquid - Google Patents
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本發明係有關於一種廢酸溶液處理方法，更特別的是一種清洗不鏽鋼、金屬或矽晶圓後之含氫氟酸之廢液處理方法。 The invention relates to a method for treating a waste acid solution, and more particularly to a method for treating a waste liquid containing hydrofluoric acid after cleaning a stainless steel, a metal or a tantalum wafer.
近年來半導體產業及液晶製造產業的蓬勃發展，相對地在製造過程中所生的廢液種類及數量也隨之增加，例如電子工業清洗製程或者平面顯示器(TFT-LCD)製程中蝕刻玻璃基板所產生的含氫氟酸廢液，因含有氫氟酸及含或不含溶解矽、硝酸、鹽酸或硫酸等不純物，無法再使用，必須當作廢水處理掉。然而這些廢水一般含有氫氟酸、硝酸、鹽酸及溶解矽等不純物，當作廢水處理時，必須耗用大量鹼來中和處理，且添加鈣鹽去除氟會產生很多微細含氟污泥，在處理上非常的困難且需要相當大的費用。此外，無法回收其中的氟有價物以得到工業上可以使用的產品，只能當作污泥處理，實在可惜又浪費資源。 In recent years, the semiconductor industry and the liquid crystal manufacturing industry have flourished, and the types and quantities of waste liquids generated in the manufacturing process have also increased. For example, in the electronic industry cleaning process or in the planar display (TFT-LCD) process, the glass substrate is etched. The produced hydrofluoric acid-containing waste liquid cannot be reused because it contains hydrofluoric acid and contains or contains impurities such as dissolved hydrazine, nitric acid, hydrochloric acid or sulfuric acid, and must be treated as waste water. However, these wastewaters generally contain impurities such as hydrofluoric acid, nitric acid, hydrochloric acid, and dissolved cesium. When treated as wastewater, a large amount of alkali must be used for neutralization treatment, and the addition of calcium salts to remove fluorine produces a lot of fine fluorine-containing sludge. It is very difficult to handle and requires considerable expense. In addition, it is impossible to recover the fluorine content in order to obtain industrially usable products, and it can only be treated as sludge, which is a waste of resources.
因此，如何將這些廢液當作廢水處理之外，又可以將其中的有價氟資源回收以供其他工業使用，是值得期待並且發展的課題。於目前一般經常採用的方法包括，係在前述的廢液中加入氫氧化鈣(Ca(OH)2)或是氯化鈣(CaCl2)，使氟離子(F-)與鈣離子(Ca2+)產生難溶於水的氟化鈣沉澱物。由於廢液中含有溶解性的二氧化矽及硫酸等不純物，因此所產生的氟化鈣沉澱物中會有二氧化矽、硫酸及鈣之共沉澱物，因此只能得到純度低 的氟化鈣，無法供應工業上使用，只能當作污泥處理，能夠創造的經濟價值不高。 Therefore, how to treat these waste liquids as wastewater treatment and recycle valuable fluorine resources for use in other industries is a problem worthy of expectation and development. The methods generally used at present include the addition of calcium hydroxide (Ca(OH)2) or calcium chloride (CaCl2) to the aforementioned waste liquid to produce fluoride ion (F-) and calcium ion (Ca2+). A calcium fluoride precipitate that is poorly soluble in water. Since the waste liquid contains impurities such as dissolved cerium oxide and sulfuric acid, the resulting calcium fluoride precipitate has a coprecipitate of cerium oxide, sulfuric acid and calcium, so that only low purity can be obtained. Calcium fluoride, which cannot be supplied for industrial use, can only be treated as sludge, and the economic value that can be created is not high.
另外，氟化鈣沉澱物非常細微，沉降速度很慢，過濾非常困難，需要很大空間的處理設備，因此相對的投資費用相當龐大，因此在處裡含有氫氟酸及含或不含溶解矽、硝酸、鹽酸或硫酸等不純物之廢液的處理上係需要一種具有經濟效益且低處理成本之廢液回收處理方法來改善目前的問題。 In addition, the calcium fluoride precipitate is very fine, the sedimentation rate is very slow, the filtration is very difficult, and it requires a large space of processing equipment, so the relative investment cost is quite large, so it contains hydrofluoric acid and contains or does not contain dissolved cesium. The treatment of waste liquids such as nitric acid, hydrochloric acid or sulfuric acid requires an economical and low-cost waste liquid recovery treatment method to improve the current problems.
本發明的主要目的在於揭露一種含氫氟酸之廢液處理方法，利用具有鹼金屬之緩衝溶液來調整含氫氟酸之廢液的酸鹼值，使得廢液中的氟離子與緩衝溶液中的鹼金屬反應，而得到高價且較高純度的氟化物，使得高價的氟化物可以供其他工業上應用。 The main object of the present invention is to disclose a method for treating a waste liquid containing hydrofluoric acid, which uses a buffer solution with an alkali metal to adjust the pH value of the waste liquid containing hydrofluoric acid, so that the fluoride ion in the waste liquid and the buffer solution are The alkali metal reacts to obtain a high-priced and relatively high-purity fluoride, so that high-priced fluoride can be used in other industries.
根據上述之目的，本發明揭露一種含氫氟酸之廢液處理方法，其包含：提供含氫氟酸之廢液；第一次調整含氫氟酸之廢液之酸鹼值之步驟，係加入第一緩衝溶液於含氫氟酸之廢液中，使得含氫氟酸之廢液之酸鹼值調整至第一酸鹼值；執行第一固液分離步驟，係將含氫氟酸之廢液進行沉澱並過濾，以將在含氫氟酸之廢液中之固體不純物濾出；執行陽離子交換處理，係將含氫氟酸之廢液中之金屬陽離子以交換方式置換；第二次調整含氫氟酸之廢液之酸鹼值步驟，係加入第二緩衝溶液於含氫氟酸之廢液中，使得含氫氟酸之廢液之酸鹼值由第一酸鹼值調整至第二酸鹼值；以及執行第二固液分離步驟，係將含氫氟酸之廢液中的固體及液體分離，以得到氟化物。 According to the above object, the present invention discloses a method for treating a waste liquid containing hydrofluoric acid, comprising: providing a waste liquid containing hydrofluoric acid; and the step of adjusting the pH value of the waste liquid containing hydrofluoric acid for the first time, Adding the first buffer solution to the waste liquid containing hydrofluoric acid, so that the pH value of the waste liquid containing hydrofluoric acid is adjusted to the first pH value; performing the first solid-liquid separation step, which is to contain hydrofluoric acid The waste liquid is precipitated and filtered to filter out the solid impurities in the waste liquid containing hydrofluoric acid; the cation exchange treatment is performed, and the metal cations in the waste liquid containing hydrofluoric acid are exchanged in an exchange manner; The step of adjusting the pH value of the waste liquid containing hydrofluoric acid is to add a second buffer solution to the waste liquid containing hydrofluoric acid, so that the pH value of the waste liquid containing hydrofluoric acid is adjusted from the first pH value to a second pH value; and performing a second solid-liquid separation step of separating the solid and the liquid in the waste liquid containing hydrofluoric acid to obtain a fluoride.
本發明之一實施例中，上述之含氫氟酸之廢液包括氫氟酸、硫酸、硝酸及鹽酸等。 In an embodiment of the invention, the waste liquid containing hydrofluoric acid comprises hydrofluoric acid, sulfuric acid, nitric acid, hydrochloric acid or the like.
本發明之一實施例中，上述之第一緩衝溶液係為氫氧化鈉溶液，其濃度範圍為10%~60%。 In one embodiment of the present invention, the first buffer solution is a sodium hydroxide solution having a concentration ranging from 10% to 60%.
本發明之一實施例中，上述之含氫氟酸之廢液之第一酸鹼值範圍為2~4。 In one embodiment of the present invention, the first pH value of the hydrofluoric acid-containing waste liquid ranges from 2 to 4.
本發明之一實施例中，上述之第一固液分離步驟係為沉澱過濾。 In an embodiment of the invention, the first solid-liquid separation step is precipitation filtration.
本發明之一實施例中，上述之陽離子交換步驟係利用鈉陽離子交換樹脂。 In one embodiment of the invention, the cation exchange step described above utilizes a sodium cation exchange resin.
本發明之一實施例中，上述之第二緩衝溶液係為氫氧化鈉溶液，其濃度範圍為10%~60%。 In one embodiment of the present invention, the second buffer solution is a sodium hydroxide solution having a concentration ranging from 10% to 60%.
本發明之一實施例中，上述之含氫氟酸之廢液之第二酸鹼值範圍為8~10。 In one embodiment of the present invention, the second pH value of the hydrofluoric acid-containing waste liquid ranges from 8 to 10.
本發明之一實施例中，上述之第二固液分離步驟係包含一過濾步驟、一脫水步驟及一烘乾步驟。 In an embodiment of the invention, the second solid-liquid separation step comprises a filtration step, a dehydration step and a drying step.
本發明之上述及其他目的與優點，不難從下述所選用實施例之詳細說明與附圖中，獲得深入了解。 The above and other objects and advantages of the present invention will be readily understood from
當然，本發明在某些另件上，或另件之安排上容許有所不同，但所選用之實施例，則於本說明書中，予以詳細說明，並於附圖中展示其構造。 Of course, the invention may be varied on certain components, or in the arrangement of the components, but the selected embodiments are described in detail in the specification and their construction is shown in the drawings.
11‧‧‧提供含氫氟酸之廢液 11‧‧‧ Providing waste liquid containing hydrofluoric acid
13‧‧‧第一次調整含氫氟酸之廢液之酸鹼值至第一酸鹼值 13‧‧‧First adjustment of the pH value of the waste liquid containing hydrofluoric acid to the first pH value
15‧‧‧第一固液分離步驟以過濾出固體不純物 15‧‧‧First solid-liquid separation step to filter out solid impurities
17‧‧‧對含氫氟酸之廢液進行陽離子交換處理 17‧‧‧Ceramic exchange treatment of waste liquid containing hydrofluoric acid
19‧‧‧第二次調整經過離子交換處理之含氫氟酸之廢液之酸鹼值至第二酸鹼值 19‧‧‧Second adjustment of the acid-base value of the ion exchange treated hydrofluoric acid-containing waste liquid to the second pH value
21‧‧‧第二固液分離步驟以得到氟化物 21‧‧‧Second solid-liquid separation step to obtain fluoride
第1圖係表示本發明所揭露之含氫氟酸之廢液處理方法之步驟流程圖。 BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the steps of a method for treating a waste liquid containing hydrofluoric acid disclosed in the present invention.
本發明在此所探討的方向為一種含氫氟酸之廢液處理方法，係將作為清洗不鏽鋼、金屬或矽晶圓表面，以去除金屬或是矽晶圓表面之氧化物之含氫氟酸之廢液進行回收，並且將這些回收後之含氫氟酸之廢液進行處理，以得到高純度的氟化物，使得這些高純度的氟化物可以供其他工業上應用。為了能徹底地瞭解本發明，將在下列的描述中提出詳盡的步驟及其組成。然而，對於本發明的較佳實施例，則會詳細描述如下，然而除了這些詳細描述之外，本發明還可以廣泛地施行在其他的實施例中，且本發明的範圍不受限定，其以之後的專利範圍為準。 The invention is directed to a method for treating a waste liquid containing hydrofluoric acid, which is used as a surface for cleaning stainless steel, metal or tantalum wafers to remove oxides of metals or oxides on the surface of the wafer. The waste liquid is recovered, and the recovered waste liquid containing hydrofluoric acid is treated to obtain a high-purity fluoride, so that these high-purity fluorides can be used in other industries. In order to thoroughly understand the present invention, detailed steps and compositions thereof will be set forth in the following description. However, the preferred embodiments of the present invention will be described in detail below, but the present invention may be widely practiced in other embodiments and the scope of the present invention is not limited by the detailed description. The scope of the patents that follow will prevail.
首先請參考第1圖。第1圖係表示本發明所揭露之含氫氟酸之廢液處理方法之步驟流程圖。在第1圖中，步驟11係為提供含氫氟酸之廢液。由於在工業製程中，在不鏽鋼、金屬或矽晶圓的表面上會有氧化物的產生，為了避免這些氧化物會影響工業製程以及最後產品的良率，在進行這些製程之前，必須要先經過一清洗步驟，以移除在不鏽鋼、金屬或矽晶圓的表面上的氧化物，其中氧化物可能是金屬氧化物例如氧化鎳(NiO2)、氧化鉻(Cr2O3)、氧化鐵(Fe2O3)等等，但不限制於此。一般來說，清洗步驟係利用酸液作為清洗溶液，例如氫氟酸或是混有氫氟酸之酸液，而半導體廠都會將這些使用過的廢液回收，再做進一步的處理。另外，在本發明的實施例中，含氫氟酸之廢液除了氫氟酸之外還可以包含硫酸、硝酸及鹽酸等 酸。 Please refer to Figure 1 first. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing the steps of a method for treating a waste liquid containing hydrofluoric acid disclosed in the present invention. In Fig. 1, step 11 is to provide a waste liquid containing hydrofluoric acid. Since there are oxides on the surface of stainless steel, metal or tantalum wafers in industrial processes, in order to avoid these oxides affecting the industrial process and the yield of the final product, it is necessary to go through these processes before proceeding. a cleaning step to remove oxides on the surface of a stainless steel, metal or tantalum wafer, where the oxide may be a metal oxide such as nickel oxide (NiO2), chromium oxide (Cr2O3), iron oxide (Fe2O3), etc. , but not limited to this. In general, the cleaning step uses an acid solution as a cleaning solution, such as hydrofluoric acid or an acid solution mixed with hydrofluoric acid, and the semiconductor plant recycles the used waste liquid for further processing. In addition, in the embodiment of the present invention, the waste liquid containing hydrofluoric acid may further contain sulfuric acid, nitric acid, hydrochloric acid, etc. in addition to hydrofluoric acid. acid.
接著於步驟13，係為第一次調整含氫氟酸之廢液之酸鹼值至第一酸鹼值。此步驟係在含氫氟酸之廢液中加入第一緩衝溶液(buffer solution)，藉由第一緩衝溶液來調整含氫氟酸之廢液的酸鹼值至第一酸鹼值，其調整後含氫氟酸之廢液之酸鹼值的範圍為pH=2~4。在本發明的實施例中，做為調整含氫氟酸之廢液的酸鹼值的第一緩衝溶液係為氫氧化鈉溶液(NaOH)，其濃度範圍為10%~60%。要說明的是，由於含氫氟酸之廢液中含有懸浮固體及溶解於含氫氟酸之廢液中的雜質，又加上在含氫氟酸之廢液都屬於強酸，都具有強腐蝕性，無法直接利用陽離子交換步驟去除在含氫氟酸之廢液中的陽離子，因此在進行陽離子交換步驟之前，必需要先調整含氫氟酸之廢液的酸鹼值。 Next, in step 13, the pH value of the waste liquid containing hydrofluoric acid is adjusted to the first pH value for the first time. In this step, a first buffer solution is added to the waste liquid containing hydrofluoric acid, and the pH value of the waste liquid containing hydrofluoric acid is adjusted to the first pH value by the first buffer solution, and the adjustment is performed. The pH of the waste liquid containing hydrofluoric acid is in the range of pH=2~4. In the embodiment of the present invention, the first buffer solution for adjusting the pH value of the waste liquid containing hydrofluoric acid is sodium hydroxide solution (NaOH), and the concentration thereof ranges from 10% to 60%. It should be noted that since the waste liquid containing hydrofluoric acid contains suspended solids and impurities dissolved in the waste liquid containing hydrofluoric acid, and the waste liquid containing hydrofluoric acid is a strong acid, it has strong corrosion. Sex, it is not possible to directly remove the cation in the waste liquid containing hydrofluoric acid by the cation exchange step, so it is necessary to adjust the pH value of the waste liquid containing hydrofluoric acid before performing the cation exchange step.
接著，步驟15係為第一固液分離步驟以得到固體不純物。由於在前述的步驟13中，含氫氟酸之廢液的酸鹼值已經藉由第一緩衝溶液來調整，所以，原本在含氫氟酸之廢液中的懸浮固體以及溶解於含氫氟酸之廢液中的雜質會因為含氫氟酸之廢液的酸鹼值的改變，而由含氫氟酸之廢液中析出變成固體不純物，且沉澱於含氫氟酸之廢液中。因此在步驟15中，係將析出的固體不純物利用過濾的方式由含氫氟酸之廢液中過濾分離出來，以降低在含氫氟酸之廢液中的不純物的含量。 Next, step 15 is a first solid-liquid separation step to obtain a solid impurity. Since in the foregoing step 13, the pH value of the waste liquid containing hydrofluoric acid has been adjusted by the first buffer solution, the suspended solid originally contained in the waste liquid containing hydrofluoric acid and dissolved in the hydrofluoric acid The impurities in the acid waste liquid are precipitated into a solid impurity from the waste liquid containing hydrofluoric acid due to the change in the pH value of the waste liquid containing hydrofluoric acid, and are precipitated in the waste liquid containing hydrofluoric acid. Therefore, in step 15, the precipitated solid impurities are separated by filtration from a waste liquid containing hydrofluoric acid to reduce the content of impurities in the waste liquid containing hydrofluoric acid.
接著，步驟17係表示對含氫氟酸之廢液進行陽離子交換處理。在此步驟17中，係將含氫氟酸之廢液通過陽離子交換樹脂例如鈉離子交換樹脂，使得在含氫氟酸之廢液中的陽離子例如鎳(Ni)、鐵(Fe)、鋁(Al)、鉻(Cr)等等可以與鈉離子交換樹脂之鈉離子(Na)進行離子交換，且由鈉離子 交換樹脂中釋放出本發明所要利用的鈉離子(Na)。 Next, step 17 represents a cation exchange treatment of the waste liquid containing hydrofluoric acid. In this step 17, the waste liquid containing hydrofluoric acid is passed through a cation exchange resin such as a sodium ion exchange resin, so that cations such as nickel (Ni), iron (Fe), and aluminum in the waste liquid containing hydrofluoric acid ( Al), chromium (Cr), etc. can be ion-exchanged with sodium ion (Na) of sodium ion exchange resin, and by sodium ion The sodium ion (Na) to be utilized in the present invention is released from the exchange resin.
接著，步驟19係表示第二次調整經過離子交換處理之含氫氟酸之廢液之酸儉值至第二酸鹼值。於前述步驟17中，經過陽離子交換處理之含氫氟酸之廢液中含有大量的鈉離子，此時為了要得到純度較高的氟化物，例如氟化鈉(NaF)，以供給工業上的使用，因此在步驟19中，係藉由做為第二緩衝溶液之氫氧化鈉溶液加入含氫氟酸之廢液中，再次將含氫氟酸之廢液的酸鹼值由第一酸鹼值調整至第二酸鹼值，此時含氫氟酸之廢液的酸鹼值範圍為係由pH=2~4調整至pH=8~10，且在調整含氫氟酸之廢液的酸鹼值的同時，可以由第二緩衝溶液所提供的鈉離子與含氫氟酸之廢液中的氟離子進行反應而產生氟化物及水溶液中其反應式如下表示：NaOH(l)+HF(l)->NaF(s)+H2O(l) Next, step 19 represents the second adjustment of the acid enthalpy value of the ion exchange treated hydrofluoric acid-containing waste liquid to the second pH value. In the foregoing step 17, the cation exchange-treated waste liquid containing hydrofluoric acid contains a large amount of sodium ions, and in order to obtain a higher purity fluoride such as sodium fluoride (NaF), it is supplied to the industrial. In use, in step 19, the sodium hydroxide solution as the second buffer solution is added to the waste liquid containing hydrofluoric acid, and the pH value of the waste liquid containing hydrofluoric acid is again from the first acid base. The value is adjusted to the second pH value. At this time, the pH value of the waste liquid containing hydrofluoric acid is adjusted from pH=2~4 to pH=8~10, and the waste liquid containing hydrofluoric acid is adjusted. At the same time of the pH value, the sodium ion provided by the second buffer solution can be reacted with the fluoride ion in the waste liquid containing hydrofluoric acid to produce a fluoride and an aqueous solution. The reaction formula is as follows: NaOH(l)+HF (l)->NaF(s)+H2O(l)
接著，步驟21係為第二固液分離步驟以得到氟化物。由前述步驟19中，所產生的氟化物係溶解於水溶液中，為了得到固體的氟化物，係再藉由固液分離步驟，其包括離心、脫水以及烘乾步驟，得到固態且具有較高純度的氟化物，這些氟化物可以進一步的可以供應給工業上使用，使得在半導體製程中的含氫氟酸之廢液有再生利用的經濟價值，另外由於氟化物以固態方式懸浮於水溶液中，因此在經過上述之固液分離步驟之後，可以輕易的將水溶液移除，而不需要有任何的廢棄物處理上的成本，大幅度的降低了含氫氟酸之廢液處理的成本以及減少環境的污染。 Next, step 21 is a second solid-liquid separation step to obtain a fluoride. In the foregoing step 19, the generated fluoride is dissolved in the aqueous solution, and in order to obtain a solid fluoride, the solid phase separation step includes a centrifugation, dehydration, and drying step to obtain a solid state and a high purity. Fluoride, which can be further supplied to industrial use, so that the hydrofluoric acid-containing waste liquid in the semiconductor process has the economic value of recycling, and since the fluoride is suspended in the aqueous solution in a solid state, After the solid-liquid separation step described above, the aqueous solution can be easily removed without any waste disposal cost, greatly reducing the cost of treating the hydrofluoric acid-containing waste liquid and reducing the environment. Pollution.
11‧‧‧提供含氫氟酸之廢液 11‧‧‧ Providing waste liquid containing hydrofluoric acid
13‧‧‧第一次調整含氫氟酸之廢液之酸鹼值至第一酸鹼值 13‧‧‧First adjustment of the pH value of the waste liquid containing hydrofluoric acid to the first pH value
15‧‧‧第一固液分離步驟以過濾出固體不純物 15‧‧‧First solid-liquid separation step to filter out solid impurities
17‧‧‧對含氫氟酸之廢液進行陽離子交換處理 17‧‧‧Ceramic exchange treatment of waste liquid containing hydrofluoric acid
19‧‧‧第二次調整經過離子交換處理之含氫氟酸之廢液之酸鹼值至第二酸鹼值 19‧‧‧Second adjustment of the acid-base value of the ion exchange treated hydrofluoric acid-containing waste liquid to the second pH value
21‧‧‧第二固液分離步驟以得到氟化物 21‧‧‧Second solid-liquid separation step to obtain fluoride
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