TWI535668B - Recycling of metal waste - Google Patents
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本發明是有關於一種金屬廢液回收處理方法，特別是指一種可達到排放水標準的金屬廢液回收處理方法。 The invention relates to a metal waste liquid recovery and treatment method, in particular to a metal waste liquid recovery and treatment method which can meet the discharge water standard.
化學鍍(Electroless plating)是利用自催化原理在基體表面沉積合金的表面處理工藝，是目前發展快速且應用範圍廣泛的一項技術。其中，化學鍍鎳因為具有耐腐蝕、表面硬度高、化學穩定性高等優點，故成為化學鍍中發展最快的一種。但因為化學鍍的製程會產生金屬廢液，若處理不當，則容易對環境生態造成嚴重的危害與汙染。因此，如何有效的處理化學鍍產生的金屬廢液則是本技術領域業者積極努力的方向。 Electroless plating is a surface treatment process that deposits an alloy on the surface of a substrate by using an autocatalytic principle. It is a technology that is rapidly developed and widely used. Among them, electroless nickel plating has become the fastest growing one in electroless plating because of its corrosion resistance, high surface hardness and high chemical stability. However, because the electroless plating process produces metal waste liquid, if it is not handled properly, it will easily cause serious damage and pollution to the environment and ecology. Therefore, how to effectively treat the metal waste liquid produced by electroless plating is a direction that the industry is actively working.
目前主要是使用沉澱法來處理化學鍍製程後所產生的金屬廢液，沉澱法係利用添加沉澱劑使該金屬廢液中的金屬離子沉澱，此法雖然可以有效地去除該金屬廢液中的金屬離子，但不僅會產生無法回收再利用的重金屬汙泥，還會造成金屬資源的浪費。此外，因為該金屬廢液中存在的有機化合物，會包覆部分的金屬離子，令該金屬廢液中的金屬離子無法完全沉澱，因此，單純添加沉澱劑處理後的該金屬廢液並無法達到環保法規的排放水標準，所以必須於添加沉澱劑後再添加氧化劑(例如：次氯酸鈉、氯氣等)氧化分解該等有機化合物，令被該有機化合物包覆的金屬離子露出，才能再進一步降低該金屬廢液中的金屬含量，使 該金屬廢液符合排放水標準。 At present, the precipitation method is mainly used to treat the metal waste liquid generated after the electroless plating process, and the precipitation method uses the precipitating agent to precipitate the metal ions in the metal waste liquid, although the method can effectively remove the metal waste liquid. Metal ions, but not only will produce heavy metal sludge that cannot be recycled, but also waste metal resources. In addition, since the organic compound present in the metal waste liquid coats part of the metal ions, the metal ions in the metal waste liquid cannot be completely precipitated. Therefore, the metal waste liquid after the simple addition of the precipitant cannot be reached. Environmental standards for discharge water standards, so it is necessary to add an oxidizing agent (for example, sodium hypochlorite, chlorine, etc.) after the addition of a precipitant to oxidize and decompose the organic compounds, so that the metal ions coated by the organic compound are exposed, and the metal can be further lowered. The metal content in the waste liquid, so that The metal waste liquid meets the discharge water standard.
然而，前述沉澱法所使用的氧化劑，由於毒性/刺激性較強，例如氯氣的毒性強，因此在操作上會有安全性的疑慮，再者，如選用的是液態的氧化劑，則會有殘留於該金屬廢液中的問題，必須再經過額外的處理才可排放。 However, the oxidizing agent used in the above precipitation method is highly toxic/irritating, for example, chlorine gas is highly toxic, so there is a safety concern in operation, and if a liquid oxidizing agent is selected, there is a residue. The problem in the metal waste liquid must be treated with additional treatment before it can be discharged.
因此，本發明之目的，即在提供一種可以使金屬廢液中的金屬含量符合排放水標準的金屬廢液回收處理方法。 Accordingly, it is an object of the present invention to provide a metal waste liquid recovery treatment method which can make the metal content in the metal waste liquid conform to the discharge water standard.
於是，本發明金屬廢液回收處理方法包含下列步驟：(i)提供一金屬廢液；(ii)在該金屬廢液中加入一第一鹼性化學品，形成一pH值不小於12的混合液；(iii)準備一臭氧微氣泡裝置，包括一臭氧產生器，及一與該臭氧產生器連接的微氣泡產生器；(iv)將自該臭氧產生器產生的臭氧通入該混合液，得到含有臭氧氣泡的混合液，再將該含有臭氧氣泡的混合液推送至該微氣泡產生器，藉由該微氣泡產生器令該臭氧氣泡細化，使該臭氧氣泡與該混合液充分混合並氧化分解該混合液中的有機化合物，以形成一反應生成液；(v)在該反應生成液中加入一第二鹼性化學品，形成一最終反應生成液；及(vi)將該最終反應生成液過濾，得到一廢液，且該廢液的金屬含量不大於1 ppm。 Therefore, the metal waste liquid recovery processing method of the present invention comprises the steps of: (i) providing a metal waste liquid; (ii) adding a first basic chemical to the metal waste liquid to form a mixture having a pH of not less than 12; (iii) preparing an ozone microbubble device comprising an ozone generator, and a microbubble generator coupled to the ozone generator; (iv) introducing ozone generated from the ozone generator into the mixture, Obtaining a mixed liquid containing ozone bubbles, and pushing the mixed liquid containing ozone bubbles to the microbubble generator, wherein the ozone bubbles are refined by the microbubble generator, and the ozone bubbles are thoroughly mixed with the mixed liquid. Oxidatively decomposing the organic compound in the mixed solution to form a reaction product; (v) adding a second basic chemical to the reaction product to form a final reaction product; and (vi) the final reaction The resulting liquid is filtered to obtain a waste liquid having a metal content of not more than 1 ppm.
有關本發明之前述及其他技術內容、特點與功效，在以下配合參考圖式之一個較佳實施例的詳細說明中，將可清楚的呈現。 The above and other technical contents, features and advantages of the present invention will be apparent from the following detailed description of the preferred embodiments.
參閱圖1，本發明金屬廢液回收處理方法的一個較佳實施例包含下列步驟： 步驟11，提供一化學鍍製程後產生的金屬廢液。 Referring to Figure 1, a preferred embodiment of the metal waste liquid recovery processing method of the present invention comprises the following steps: Step 11 provides a metal waste liquid produced after an electroless plating process.
步驟12，在該金屬廢液中加入一第一鹼性化學品，形成一pH值不小於12的混合液。該第一鹼性化學品選自氫氧化鈉、氫氧化鉀、氫氧化鈣，及鹼金鹼土族的鹼性化學品，利用該第一鹼性化學品與該金屬廢液中大部分的金屬離子反應，生成金屬氫氧化物沉澱物。 In step 12, a first alkaline chemical is added to the metal waste liquid to form a mixed liquid having a pH of not less than 12. The first alkaline chemical is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, and an alkaline alkali metal alkaline chemical, and the first alkaline chemical and the metal of the metal waste liquid are utilized. The ion reacts to form a metal hydroxide precipitate.
步驟13，準備一如圖2所示的臭氧微氣泡裝置，包括一容槽2、一回流式幫浦3、一臭氧產生器4，及一微氣泡產生器5；該回流式幫浦3、該臭氧產生器4，及該微氣泡產生器5依序與該容槽2連接。此外，該臭氧微氣泡裝置還包括一壓力偵測器6、一壓力調整器7，及一溫度控制器8，該壓力調整器7及該溫度控制器8分別與該容槽2連接，藉由該壓力偵測器6偵測該容槽2的壓力，並由該壓力調整器7控制該容槽2的壓力，可避免該金屬廢液回收處理過程中不斷產生的氣體導致該容槽2壓力過大的問題，而該溫度控制器8則可使容置於該容槽2的液體維持在一設定溫度，以利反應進行。 Step 13, preparing an ozone microbubble device as shown in FIG. 2, comprising a cuvette 2, a reflow type pump 3, an ozone generator 4, and a microbubble generator 5; the reflow type pump 3 The ozone generator 4 and the microbubble generator 5 are sequentially connected to the tank 2. In addition, the ozone microbubble device further includes a pressure detector 6, a pressure regulator 7, and a temperature controller 8, and the pressure regulator 7 and the temperature controller 8 are respectively connected to the tank 2, by The pressure detector 6 detects the pressure of the tank 2, and the pressure of the tank 2 is controlled by the pressure regulator 7, so that the gas generated in the metal waste liquid recovery process can be prevented from causing the pressure of the tank 2 Excessive problem, and the temperature controller 8 can maintain the liquid contained in the tank 2 at a set temperature for the reaction to proceed.
步驟14，將該混合液置於該容槽2中，利用該回流式幫浦3將該混合液往該臭氧產生器4輸送，令自該臭氧產 生器4產生的臭氧與該混合液混合，形成一含有臭氧氣泡的混合液；接著再將該含有臭氧氣泡的混合液推送至該微氣泡產生器5，藉由該微氣泡產生器5進而將該混合液中的臭氧氣泡粉碎形成超微細的臭氧氣泡。藉由形成超微細的臭氧氣泡增加該些臭氧氣泡與該混合液的接觸面積，而可更有效的將該混合液中的有機化合物氧化分解，使被該有機化合物包覆的金屬離子露出，以形成一反應生成液。 Step 14, the mixed liquid is placed in the tank 2, and the mixed liquid is sent to the ozone generator 4 by the reflux pump 3, and the ozone is produced from the ozone. The ozone generated by the burner 4 is mixed with the mixed liquid to form a mixed liquid containing ozone bubbles; then the mixed liquid containing ozone bubbles is pushed to the microbubble generator 5, and the microbubble generator 5 is further The ozone bubbles in the mixture are pulverized to form ultrafine ozone bubbles. By forming ultrafine ozone bubbles to increase the contact area between the ozone bubbles and the mixed solution, the organic compound in the mixed solution can be more efficiently oxidized and decomposed, and the metal ions coated by the organic compound are exposed. A reaction product is formed.
要說明的是，該步驟14的反應過程中，該壓力調整器7是控制在1.5至1.7(kg/cm2)，而為了提升臭氧與該有機化合物間的氧化分解反應速率，較佳地，該混合液的溫度係維持在50℃至90℃。 It is to be noted that, in the reaction of the step 14, the pressure regulator 7 is controlled at 1.5 to 1.7 (kg/cm 2 ), and in order to increase the rate of oxidative decomposition reaction between the ozone and the organic compound, preferably, The temperature of the mixture is maintained at 50 ° C to 90 ° C.
步驟15，接著，在該反應生成液中加入一第二鹼性化學品，形成一最終反應生成液。該第二鹼性化學品選自氫氧化鈉、氫氧化鉀、氫氧化鈣，及鹼金鹼土族的鹼性化學品，利用該第二鹼性化學品進一步與該反應生成液中的金屬離子反應，生成金屬氫氧化物沉澱物。 In step 15, a second basic chemical is added to the reaction product to form a final reaction product. The second alkaline chemical is selected from the group consisting of sodium hydroxide, potassium hydroxide, calcium hydroxide, and an alkaline alkali metal alkaline chemical, and the second basic chemical is further used to further metal ions in the reaction liquid. The reaction produces a metal hydroxide precipitate.
此外，要說明的是，該步驟15中所加入的該第二鹼性化學品與該步驟12中加入的該第一鹼性化學品可為相同或不同。 In addition, it is to be noted that the second alkaline chemical added in the step 15 may be the same as or different from the first basic chemical added in the step 12.
步驟16，將該最終反應生成液過濾，得到一過濾物，及一金屬含量不大於1 ppm的廢液。將所得的該過濾物進行水洗純化，即得到可回收再利用的金屬氫氧化物，且該廢液的金屬含量亦符合環保法規的排放水標準。 In step 16, the final reaction product is filtered to obtain a filtrate and a waste liquid having a metal content of not more than 1 ppm. The obtained filtrate is subjected to water washing and purification to obtain a metal hydroxide which can be recycled and reused, and the metal content of the waste liquid also meets the discharge water standard of environmental protection regulations.
本發明將就以下2個具體例及2個比較例作進一步說 明，但該等具體例僅為說明之用，不應被解釋為本發明實施的限制。 The present invention will further elaborate on the following two specific examples and two comparative examples. The specific examples are for illustrative purposes only and should not be construed as limiting the invention.
(1-1)分別提供3L經化學鍍製程後未經處理的化鎳廢液，且該化鎳廢液中鎳含量為5553 ppm。 (1-1) Providing 3L of untreated nickel waste liquid after the electroless plating process, and the nickel content in the nickel waste liquid is 5553 ppm.
(1-2)分別在該等化鎳廢液中加入不同的鹼性化學品，該鹼性化學品選自氫氧化鈉、氫氧化鉀，及氫氧化鈣，以分別形成pH值為12.5的混合液。 (1-2) separately adding different alkaline chemicals to the nickel waste liquid, the alkaline chemicals being selected from the group consisting of sodium hydroxide, potassium hydroxide, and calcium hydroxide to form a pH of 12.5, respectively. Mixture.
(1-3)將該等混合液分別置於該臭氧微氣泡裝置的容槽2中，並使該等混合液的溫度維持在70℃，令臭氧與該等混合液混合，形成溶有臭氧氣泡的混合液，接著再推送至該微氣泡產生器5，使該等混合液中的臭氧氣泡粉碎形成超微細的臭氧氣泡，反應時間為3小時，分別形成反應生成液。 (1-3) separately placing the mixed liquids in the tank 2 of the ozone microbubble device, and maintaining the temperature of the mixed liquid at 70 ° C to mix ozone with the mixed liquid to form dissolved ozone The mixed liquid of the bubbles was further pushed to the microbubble generator 5, and the ozone bubbles in the mixed liquid were pulverized to form ultrafine ozone bubbles, and the reaction time was 3 hours to form a reaction product liquid.
(1-4)在該等反應生成液中加入與步驟(1-2)相同的鹼性化學品，以分別形成pH值為12.5的最終反應生成液。 (1-4) The same basic chemicals as in the step (1-2) were added to the reaction product liquids to form a final reaction product liquid having a pH of 12.5, respectively.
(1-5)將該等最終反應生成液過濾，分別得到氫氧化鎳沉澱物及廢液。 (1-5) The final reaction product liquid was filtered to obtain a nickel hydroxide precipitate and a waste liquid, respectively.
其中，以臭氧當作氧化劑參與反應，並藉由該微氣泡產生器5有效地增加臭氧與該混合液的接觸面積，就加入鹼性化學品的不同，該等氫氧化鎳回收率及該等廢液中鎳含量的分析結果如下表所示：
(2-1)分別提供3L經化學鍍製程後未經處理的化鎳廢液，且該化鎳廢液中鎳含量為5553 ppm。 (2-1) 3L of untreated nickel waste liquid after electroless plating is separately provided, and the nickel content in the nickel waste liquid is 5553 ppm.
(2-2)分別在該等化鎳廢液中加入氫氧化鈉，以分別形成pH值為12.5的混合液。 (2-2) Sodium hydroxide was added to the nickel waste liquid to form a mixed liquid having a pH of 12.5, respectively.
(2-3)將該等混合液分別置於該臭氧微氣泡裝置的容槽2中，並使該等混合液的溫度分別維持在50℃及90℃，令臭氧與該等混合液混合，形成溶有臭氧氣泡的混合液，接著再推送至該微氣泡產生器5，使該等混合液中的臭氧氣泡粉碎形成超微細的臭氧氣泡，反應時間為3小時，分別形成反應生成液。 (2-3) separately disposing the mixed liquid in the tank 2 of the ozone microbubble device, and maintaining the temperature of the mixed liquid at 50 ° C and 90 ° C, respectively, so that ozone is mixed with the mixed liquid. A mixed liquid in which ozone bubbles were dissolved was formed, and then pushed to the microbubble generator 5 to pulverize the ozone bubbles in the mixed liquid to form ultrafine ozone bubbles, and the reaction time was 3 hours to form a reaction product liquid.
(2-4)在該等反應生成液中加入氫氧化鈉，分別形成pH值為12.5的最終反應生成液。 (2-4) Sodium hydroxide was added to the reaction product liquids to form a final reaction product liquid having a pH of 12.5.
(2-5)將該等最終反應生成液過濾，分別得到氫氧化鎳沉澱物及廢液。 (2-5) The final reaction product liquid was filtered to obtain a nickel hydroxide precipitate and a waste liquid, respectively.
其中，以臭氧當作氧化劑參與反應，並藉由該微氣泡產生器5有效地增加臭氧與該混合液的接觸面積，就反應溫度的不同，該等氫氧化鎳回收率及該等廢液中鎳含量的分析結果如下表所示：
(1-1)分別提供3L經化學鍍製程後未經處理的化鎳廢液，且該化鎳廢液中鎳含量為5553 ppm。 (1-1) Providing 3L of untreated nickel waste liquid after the electroless plating process, and the nickel content in the nickel waste liquid is 5553 ppm.
(1-2)分別在該等化鎳廢液中加入不同的鹼性化學品，該鹼性化學品選自氫氧化鈉、氫氧化鉀，及氫氧化鈣，以分別形成pH值為12.5的混合液。 (1-2) separately adding different alkaline chemicals to the nickel waste liquid, the alkaline chemicals being selected from the group consisting of sodium hydroxide, potassium hydroxide, and calcium hydroxide to form a pH of 12.5, respectively. Mixture.
(1-3)將該等混合液過濾，分別得到氫氧化鎳沉澱物及廢液。 (1-3) The mixed liquid was filtered to obtain a nickel hydroxide precipitate and a waste liquid, respectively.
其中，無添加氧化劑參與反應就加入鹼性化學品的不同，該等氫氧化鎳回收率及該等廢液中鎳含量的分析結果如下表所示：
(2-1)分別提供3L經化學鍍製程後未經處理的化鎳廢液，且該化鎳廢液中鎳含量為5553 ppm。 (2-1) 3L of untreated nickel waste liquid after electroless plating is separately provided, and the nickel content in the nickel waste liquid is 5553 ppm.
(2-2)分別在該等化鎳廢液中加入氫氧化鈉，以分別形成pH值為12.5的混合液。 (2-2) Sodium hydroxide was added to the nickel waste liquid to form a mixed liquid having a pH of 12.5, respectively.
(2-3)使該等混合液溫度維持在30℃，分別加入過氧化氫及次氯酸鈉當作氧化劑，反應時間為3小時，分別形成反應生成液。 (2-3) The temperature of the mixed solution was maintained at 30 ° C, and hydrogen peroxide and sodium hypochlorite were respectively added as an oxidizing agent, and the reaction time was 3 hours to form a reaction product liquid, respectively.
(2-4)在該等反應生成液中加入氫氧化鈉，以分別形成 pH值為12.5的最終反應生成液。 (2-4) adding sodium hydroxide to the reaction liquids to form separately The final reaction product having a pH of 12.5.
(2-5)將該等最終反應生成液過濾，分別得到氫氧化鎳沉澱物及廢液。 (2-5) The final reaction product liquid was filtered to obtain a nickel hydroxide precipitate and a waste liquid, respectively.
其中，就加入氧化劑的不同，該等氫氧化鎳回收率及該等廢液中鎳含量的分析結果如下表所示：
歸納上述結果顯示，對於處理化學鍍製程後所產生的金屬廢液，比較該等具體例及該等比較例可發現，該比較例1無添加氧化劑進行反應，該等廢液中的鎳含量皆無法達到1 ppm以下的排放水標準；而該比較例2分別使用過氧化氫及次氯酸鈉當作氧化劑，氧化分解該化鎳廢液中的有機化合物，由分析結果顯示，使用該過氧化氫及該次氯酸鈉作為氧化劑，雖然已可有效降低該化鎳廢液中的鎳含量，但還是無法達到排放水的標準，且液態的氧化劑亦會殘留於該化鎳廢液中，必須再經過額外的處理才可排放。 The above results show that, for the metal waste liquid generated after the electroless plating process, comparing the specific examples and the comparative examples, it can be found that the comparative example 1 has no oxidizing agent for reaction, and the nickel content in the waste liquids is The discharge water standard of 1 ppm or less could not be reached; and in Comparative Example 2, hydrogen peroxide and sodium hypochlorite were respectively used as oxidants to oxidatively decompose the organic compound in the nickel waste liquid, and the analysis showed that the hydrogen peroxide was used and Sodium hypochlorite as an oxidant, although it can effectively reduce the nickel content in the nickel waste liquid, it still cannot meet the discharge water standard, and the liquid oxidant will remain in the nickel waste liquid, and must be subjected to additional treatment. Can be discharged.
然而，該具體例1及該具體例2是使用臭氧作為氧化劑參與反應，並藉由該微氣泡產生器5將臭氧氣泡細化形成超微細的臭氧氣泡，有效地增加臭氧與該混合液的接觸面積，由分析結果顯示，該化鎳廢液中的鎳含量已大幅下降且皆在0.5 ppm以下，符合環保法規的排放水標準。此外，由該具體例2可知，反應溫度的增加確實可使臭氧與該有機化合物間的氧化分解反應速率提升，進而有效地降 低該化鎳廢液中的鎳含量。再者，氣態的臭氧在使用過後會分解成為氧氣，不具有毒性亦不會對該化鎳廢液造成任何影響。 However, in the specific example 1 and the specific example 2, ozone is used as an oxidizing agent to participate in the reaction, and the microbubble generator 5 refines the ozone bubbles to form ultrafine ozone bubbles, thereby effectively increasing the contact of the ozone with the mixed solution. According to the analysis results, the nickel content in the nickel waste liquid has been greatly reduced and both are below 0.5 ppm, which meets the discharge water standards of environmental regulations. Further, as is apparent from the specific example 2, the increase in the reaction temperature actually increases the rate of oxidative decomposition reaction between ozone and the organic compound, thereby effectively lowering Low nickel content in the nickel waste liquid. Furthermore, gaseous ozone decomposes into oxygen after use, and it is not toxic and does not have any effect on the nickel waste liquid.
綜上所述，本發明使用臭氧當作氧化劑，並利用該微氣泡產生器5有效地增加臭氧與該金屬廢液的接觸面積與滯留時間，加強反應進行並充分氧化分解存在於該金屬廢液中的有機化合物，進而使該金屬廢液中的金屬含量降低達到排放水的標準，故確實能達成本發明之目的。 In summary, the present invention uses ozone as an oxidant, and utilizes the microbubble generator 5 to effectively increase the contact area and residence time of ozone with the metal waste liquid, strengthen the reaction, and fully oxidize and decompose in the metal waste liquid. The organic compound in the process further reduces the metal content in the metal waste liquid to the standard of discharged water, so that the object of the present invention can be achieved.
惟以上所述者，僅為本發明之較佳實施例而已，當不能以此限定本發明實施之範圍，即大凡依本發明申請專利範圍及發明說明內容所作之簡單的等效變化與修飾，皆仍屬本發明專利涵蓋之範圍內。 The above is only the preferred embodiment of the present invention, and the scope of the invention is not limited thereto, that is, the simple equivalent changes and modifications made by the scope of the invention and the description of the invention are All remain within the scope of the invention patent.
2‧‧‧容槽 2‧‧‧ 容容
3‧‧‧回流式幫浦 3‧‧‧Reflow pump
4‧‧‧臭氧產生器 4‧‧‧Ozone generator
5‧‧‧微氣泡產生器 5‧‧‧Microbubble generator
6‧‧‧壓力偵測器 6‧‧‧ Pressure detector
7‧‧‧壓力調整器 7‧‧‧Pressure regulator
8‧‧‧溫度控制器 8‧‧‧ Temperature Controller
圖1是一流程圖，說明本發明金屬廢液回收處理方法的一較佳實施例；及圖2是一用以實施本發明金屬廢液回收處理方法的裝置構成圖。 BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a flow chart showing a preferred embodiment of a metal waste liquid recovery processing method of the present invention; and Fig. 2 is a view showing a configuration of a device for carrying out the metal waste liquid recovery processing method of the present invention.
2‧‧‧容槽 2‧‧‧ 容容
3‧‧‧回流式幫浦 3‧‧‧Reflow pump
4‧‧‧臭氧產生器 4‧‧‧Ozone generator
5‧‧‧微氣泡產生器 5‧‧‧Microbubble generator
6‧‧‧壓力偵測器 6‧‧‧ Pressure detector
7‧‧‧壓力調整器 7‧‧‧Pressure regulator
8‧‧‧溫度控制器 8‧‧‧ Temperature Controller
Claims (5)
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| TW101135917A TWI535668B (en) | 2012-09-28 | 2012-09-28 | Recycling of metal waste |
| CN201210393855.6A CN103708639A (en) | 2012-09-28 | 2012-10-17 | Metal waste liquid recovery treatment method |
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| TW101135917A TWI535668B (en) | 2012-09-28 | 2012-09-28 | Recycling of metal waste |
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