TW574059B - Method for recovering high purity salt from waste solution of salting-out of dye - Google Patents
Method for recovering high purity salt from waste solution of salting-out of dye Download PDFInfo
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574059 五、發明說明(1) 本發明係有關於一種自染料鹽析廢液回收高純度鹽的 方法,特別是指利用蒸發結晶及電解氧化等步驟而回收製 得高純度氯化納或氯化鉀晶體,且無二次污染產生者。 按,在一般的染料生產過程中,特別是反應性染料及 直接染料,在反應合成後,常須使用鹽析法使染料因溶解 度降低而沉澱或結晶析出,為求提高染料回收率,須添加 大量的氯化鈉或氯化鉀等無機鹽類來進行染料鹽析,在過 濾取得染料作為產品後,留下含有高濃度無機鹽類的廢液 須予以妥善處理。廢液中含5〜30%氯化鈉或氯化鉀、 0 . 3〜2 . 0 w t %染料及其中間體,ρ Η值介於1到1 2,透視度極 低。 對於這些廢液的處理,目前習用方法為利用稀釋、化 學混凝、生物分解等步驟的組合,但有生物分解效率低及 有機污泥二次污染等問題,且未回收無機鹽類再利用; 亦有利用液體直接焚化法處理高鹽份廢液者(染料鹽 析廢液屬於高鹽份廢液),但因氯化鈉及氯化鉀於高溫焚 化過程中會分解產生氧化鈉、氧化鉀、氯氣等高腐蝕性物 質,造成設備維修費用過高的問題,且亦難以回收無機鹽 類再利用; 對於環氧樹脂廠及聚碳酯廠所產生的高鹽份廢液,目 前有採用旋轉窯法者,其首先對廢液進行蒸發結晶,結晶 所得氯化鈉晶體利用旋轉窯爐在7 0 0〜1 0 0 0 °C的高溫下將晶β1 體表面的有機物予以氧化或碳化,但因氣化鈉晶體的熔點 為8 0 1 °C,旋轉窯爐溫度超過8 0 1 °C即會使氣化鈉晶體熔解574059 V. Description of the invention (1) The present invention relates to a method for recovering high-purity salts from a dye salting-out waste liquid, in particular to recovering and obtaining high-purity sodium chloride or chlorination through steps such as evaporation crystallization and electrolytic oxidation. Potassium crystals without secondary pollution. According to the general dye production process, especially reactive dyes and direct dyes, after the synthesis of the reaction, the salting out method must be used to make the dye precipitate or crystallize due to the reduced solubility. In order to improve the dye recovery rate, it is necessary to add A large number of inorganic salts such as sodium chloride or potassium chloride are used for dye salting out. After the dye is obtained as a product by filtration, the waste liquid containing high concentration of inorganic salts must be properly treated. The waste liquid contains 5 ~ 30% sodium chloride or potassium chloride, 0.3 ~ 2.0 w t% dye and its intermediate, ρ Η value is between 1 and 12, and the perspective is extremely low. For the treatment of these waste liquids, the current conventional method is to use a combination of steps such as dilution, chemical coagulation, and biological decomposition, but it has problems such as low biological decomposition efficiency and secondary pollution of organic sludge, and the inorganic salts are not recovered for reuse; There are also those who use liquid direct incineration to treat high-salt waste liquid (dye salting-out waste liquid is a high-salt waste liquid), but sodium chloride and potassium chloride will decompose during the high temperature incineration process to produce sodium oxide and potassium oxide. Highly corrosive substances, such as chlorine and chlorine gas, cause the problem of high equipment maintenance costs, and it is difficult to recycle inorganic salts for reuse. For the high-salt waste liquid produced by epoxy resin plants and polycarbonate plants, rotation is currently used. The kiln method first evaporates and crystallizes the waste liquid. The sodium chloride crystals obtained from the crystallization are oxidized or carbonized on the surface of the crystal β1 body by a rotary kiln at a high temperature of 700 to 100 ° C. Since the melting point of sodium gasified crystals is 80 1 ° C, the temperature of the rotary kiln exceeding 80 1 ° C will melt the sodium gasified crystals.
574059 五、發明說明(2) 並包入有機物,使得無法將有機物完全氧化或碳化,導致 回收的氣化納晶體純度不兩, 另於中華民國專利公告號2 2 3 0 44,標題為「由高濃度 鹽類之廢水中回收鹽類之方法」中,其教導利用蒸發結晶 法使氯化鈉或氯化鉀自廢液中結晶析出,再以紅外線產生 器發出6 0 0〜3 0 0 0 °C的高溫紅外線將晶體表面的有機物予以 氧化或碳化,之後進行再結晶以製得高純度氯化鈉或氯化 鉀晶體,須運用到6 0 0〜3 0 0 0 °C的高溫紅外線及紅外線處理 後的晶體須進行再結晶方能回收高純度的無機鹽類為此方 法之主要缺點。 為改善習用技術之缺點,本發明人憑其從事相關產業4 之多年經驗,竭盡心智,終有本發明之產生。於是,本發 明一種由染料鹽析廢液回收高純度鹽的方法,無須在高溫 下將晶體表面有機物予以氧化或碳化,亦不須進行再結 晶,即能製得高純度無機鹽晶體且無有機污泥二次污染之 問題。 因此,本發明之目的為提供一種由染料鹽析廢液回收 高純度鹽的方法。 為達上述目的,本發明是這樣實現的: 一種由染料鹽析廢液回收高純度鹽的方法,係包括 (1) 進行蒸發濃縮,使廢液中所含氯化鈉或氯化鉀等無機 鹽類因過飽和而結晶析出; ® (2) 過濾蒸發結晶所得溼晶體,添加後續步驟回收之鹽液 使形成懸浮液,利用電解氧化法將晶體表面附著之染574059 V. Description of the invention (2) The inclusion of organic matter makes it impossible to completely oxidize or carbonize the organic matter, which results in the purity of the recovered vaporized sodium crystals being the same. It is also disclosed in the Republic of China Patent Publication No. 2 2 3 0 44, entitled "The method of recovering salt from wastewater with high concentration of salt" teaches the use of evaporative crystallization to crystallize sodium chloride or potassium chloride from waste liquid, and then emit it from an infrared generator 6 0 0 ~ 3 0 0 0 The high temperature infrared of ° C will oxidize or carbonize the organic compounds on the surface of the crystal, and then recrystallize to obtain high-purity sodium chloride or potassium chloride crystals. The high temperature infrared of 600 ° C ~ 300 ° C The main disadvantage of this method is that the crystals after infrared treatment must be recrystallized to recover high-purity inorganic salts. In order to improve the shortcomings of the conventional technology, the inventor relied on his many years of experience in related industries, and devoted his mind to the invention. Therefore, the method for recovering high-purity salts from the dye salting-out waste liquid of the present invention does not need to oxidize or carbonize organic substances on the surface of the crystal at high temperature, and does not need to recrystallize. The problem of secondary pollution of sludge. Therefore, an object of the present invention is to provide a method for recovering a high-purity salt from a dye salting-out waste liquid. In order to achieve the above object, the present invention is achieved as follows: A method for recovering high-purity salts from a dye salting-out waste liquid, which comprises (1) evaporating and concentrating the inorganic liquid such as sodium chloride or potassium chloride contained in the waste liquid Salts crystallize due to supersaturation; ® (2) Filter the wet crystals obtained by evaporation and crystallization, add the salt solution recovered in the subsequent steps to form a suspension, and use electrolytic oxidation to attach the dye on the surface of the crystals.
第5頁 574059 五、發明說明(3) 料及其中間體 等有機物予以氧化分解; (3 )過濾及乾燥晶體,過濾之鹽液回流再使用等步驟。 為使 貴審查委員瞭解本發明之目的、特徵及功效, 茲藉由下述具體之實施例,並配合所附之圖式,對本發明 做一詳細說明,說明如后: 實施例1 請參閱第一圖,係為本發明一種由染料鹽析廢液回收 高純度鹽的方法之處理流程圖,如圖所示:在進行本處理 前,染料鹽析廢液1的pH值低於4或高於10,須先將廢液 中和2 ,利用鹽酸液、氫氧化鈉液或氫氧化鉀液中和2廢 液至pH值介於4〜1 0之間。於真空或常壓下進行蒸發結晶 4 3 ,適合操作條件為50〜110°C、30torr〜latm,蒸發結晶 3過程中只要確保結晶槽中之晶體含量達到1 〇 vo 1. %以 上,即易於使氯化鈉或氣化鉀結晶成完整晶體,亦即有機 雜質不被包入晶體中而僅附著在晶體表面。於蒸發結晶3 過程中,餾出的冷凝液4 ,可再回收使用,無二次污染問 題;廢液中所含有機物亦會沉澱或結晶析出而浮於結晶槽 液面,其於上層形成有機懸浮物5 ,取出作為次級染料6 或予以焚化7 。蒸發結晶3後所得懸浮液8經過濾9後, 其濾液1 0經回流1 1至蒸發結晶槽,濕晶體1 2經加入 新鮮鹽液或回收鹽液1 3使形成懸浮液1 4,濕晶體1 2 與鹽液之體積比以介於1 ·· 0. 5〜2 0之間較佳,以懸浮液1 ® 4能適度攪動為原則。將懸浮液1 4置入電解槽中,陽極 板材質較佳為貴金屬,亦可使用不銹鋼或石墨等;而陰極Page 5 574059 V. Description of the invention (3) Organic materials such as materials and intermediates are oxidized and decomposed; (3) Filtering and drying the crystals, filtering salt solution is refluxed and then used. In order for your reviewing committee to understand the purpose, features and effects of the present invention, the following specific examples are given in conjunction with the accompanying drawings to make a detailed description of the present invention, as described below: Example 1 A figure is a processing flow chart of a method for recovering high-purity salts from a dye salting-out waste liquid according to the present invention. As shown in the figure: before the treatment, the pH value of the dye salting-out waste liquid 1 is lower than 4 or high. At 10, the waste liquid must be neutralized 2 and the waste liquid 2 is neutralized with hydrochloric acid solution, sodium hydroxide solution or potassium hydroxide solution to a pH value between 4 and 10. Evaporation and crystallization 4 3 under vacuum or normal pressure, suitable operating conditions are 50 ~ 110 ° C, 30torr ~ latm. During the process of evaporation crystallization 3, as long as the crystal content in the crystallization tank is more than 1 vo 1.%, it is easy. Crystallize sodium chloride or potassium gas into complete crystals, that is, organic impurities are not enclosed in the crystals, but only adhere to the surface of the crystals. In the process of evaporation and crystallization 3, the condensate 4 distilled off can be reused without secondary pollution; the organic substances contained in the waste liquid will also precipitate or crystallize out and float on the liquid surface of the crystallization tank, which forms organics in the upper layer. Suspended matter 5 is removed as secondary dye 6 or incinerated 7. The suspension 8 obtained after evaporating the crystal 3 was filtered 9 and the filtrate 10 was refluxed 11 to the evaporation crystallization tank. Wet crystals 12 were added to fresh salt solution or recovered salt solution 1 3 to form suspension 14 and wet crystals. The volume ratio of 1 2 to the salt solution is preferably between 1. · 0.5 to 2 0, and the suspension 1 1 4 can be moderately agitated as a principle. Put the suspension 14 into the electrolytic cell. The anode plate is preferably made of precious metal, and stainless steel or graphite can also be used. The cathode
574059 五、發明說明(4) 板材質較佳為主 氧化1 5期μ # , 了使用不銹鋼或銅等;進行電解 較佳者為40〜95(Γ〇γ持懸广·液1 4溫度在室溫至100。〇之間, 間,較佳是^ Q C之間,陰陽極之電位差保持在卜1 5 V之 1 4予以~ m〜5 V之間;電解氧化1 5過程中須對懸浮液 4予以劇烈擾拌。電解過程中之陰陽極反應式如下: 陽極(氧化反應): 2 C 1 ► C 1 2 十 2 e - 陰極(還原反應): 礓1 2Na十十 2H2〇 十 2 e一->2 Na OH+ H2t 或 2K十十2H2〇十2e 一 一〜► 2KOH十H2t 由於對懸浮液1 4劇烈攪拌,陽極產生的氯氣會與陰 極產生的氩氧化鈉或氫氧化鉀反應形成次氣酸鈉及氯酸鈉· 或次氣酸鉀及氯酸鉀,反應式如下:574059 V. Description of the invention (4) The material of the plate is preferably the main oxidation phase 15 μ #, using stainless steel or copper, etc .; electrolysis is preferably 40 ~ 95 (Γ〇γ Between room temperature and 100 °, preferably between ^ QC, the potential difference between the cathode and anode is maintained between 14 and 15 ~ 15 ~ 5 V; the suspension must be suspended during electrolytic oxidation 15 4 Stir and stir vigorously. The reaction formula of cathode and anode during electrolysis is as follows: anode (oxidation reaction): 2 C 1 ► C 1 2 ten 2 e-cathode (reduction reaction): 礓 1 2Na ten ten 2H20 ten two e one -> 2 Na OH + H2t or 2K ten ten 2H2 0 ten 2e one to one ► ► 2KOH ten H2t As the suspension 14 is stirred vigorously, the chlorine gas produced by the anode will react with the sodium argon oxide or potassium hydroxide produced by the cathode to form secondary Sodium gas and sodium chlorate · or potassium hypochlorite and potassium chlorate, the reaction formula is as follows:
第7頁 574059 五、發明說明(5)Page 7 574059 V. Description of the invention (5)
Cl2 十 2NaOH 十 1/2〇2-N a C 1 0 + H2〇Cl2 ten 2NaOH ten 1/20 2-N a C 1 0 + H2〇
Cl2 十 2Na〇H十 5/2〇2-►δΝ a C 1 03 + H2〇 或 C l2 + 2KOH+ l/2〇2-KC 1 o + h2o C 12十 2K〇H+5/2〇2 ——-2KC 1 o3 + h2o 因電解產生的氣氣、次氯酸鈉及氯酸鈉亦或次氯酸鉀 及氯酸鉀等強氧化劑可對附著在氣化鈉或氯化鉀晶體表面 的有機物予以有效氧化分解。當電解至懸浮液1 4中之溶 液成為無色透明時,過濾1 6懸浮液1 4 ,其濾液1 7 (鹽液)經回流1 8再使用,而濕晶體1 9則經乾燥2 0即 可製得高純度氯化鈉或氣化鉀晶體2 1 。 實施例2 取3 0 0 0ml淡褐色染料鹽析廢液,廢液pH值1. 18,内含 0 · 6 2 %染料及其中間體等有機物與1 3 · 9 7 %氣化鈉。以氫氧 化鈉中和至p Η為5 · 8,於常壓、1 0 3〜1 0 7 °C條件下進行蒸發 結晶,餾出22 0 0ml冷凝液,冷凝液pH值為5. 45,内含 丨 4 4 p p m氣化鈉,另殘留約8 0 0 m 1含氣化鈉晶體的懸浮液。經 過濾得表面帶褐色的濕氯化納晶體,添加5 0 0 in 1飽和鹽Cl2 ten 2Na〇H ten 5 / 2〇2-►δΝ a C 1 03 + H2〇 or C l2 + 2KOH + l / 2〇2-KC 1 o + h2o C 12 ten 2K〇H + 5 / 2〇2 — —-2KC 1 o3 + h2o Gas produced by electrolysis, sodium hypochlorite and sodium chlorate, or strong oxidants such as potassium hypochlorite and potassium chlorate can effectively oxidize and decompose the organic matter attached to the surface of sodium vapor or potassium chloride crystals. When the solution in the suspension 14 is electrolyzed to become colorless and transparent, 16 suspensions 14 are filtered, and the filtrate 17 (salt solution) can be reused after refluxing 18, and the wet crystals 19 can be dried and dried. High-purity sodium chloride or potassium gas crystals 2 1 were obtained. Example 2 Take 3 0 0 ml of light brown dye salting waste liquid, the pH of the waste liquid is 1. 18, containing 0.62% organic matter such as dyes and intermediates, and 13.97% sodium gasification. 45 , Neutralize with sodium hydroxide until p Η is 5 · 8, evaporate and crystallize at atmospheric pressure, 103 ~ 107 ° C, and distill off 2 200ml condensate, the condensate pH is 5.45, Contains 4 ppm sodium vaporized sodium, and about 800 m 1 of the suspension containing sodium vaporized crystals remains. Filtered to obtain brown wet sodium chloride crystals on the surface, adding 50 0 in 1 saturated salt
第8頁 574059 五、發明說明(6) 液’於4 5〜5 C_、陰陽極電位差為5 v的條件下進行電解氧 化’ 3 0分鐘後洛液成為無色透明,經過濾、乾燥得2 3 5 g純 度為9 9 · 5 7 %的白色氣化鈉晶體,其純度高於A c s試藥級標 準 9 9 . 5 0 °/〇。 實施例3 取3 0 0 0ml濃紫藍色染料鹽析廢液,廢液pH值8 · 91,内 含1 · 64%染料及。其中間體等有機物與丨6· 〇〇%氯化鈉。於 80torr、60〜6 5 °C條件下進行蒸發結晶,餾出2〇〇〇ml冷凝 液’冷凝液pH值為7· 85,内含6· 5 ppm氯化鈉,另殘留約 1 0 0 0 m 1含氣化納晶體的懸浮液。經過濾得表面帶紫藍色的 濕乳化納體’添加3 〇 〇 η 1飽和鹽液,於4 〇〜4 5 °C、陰陽極 電位差為4 V的條件下進行電解氧化,6 〇分鐘後溶液成為無 色透明’經過濾、乾燥得2 2 〇 g純度為9 9 . 5 2 %的白色氯化鈉 晶體。 實施例4 取2 0 0 0 ml濃紫色染料鹽析廢液,廢液pH值4· 78,内含 1 · 3 4 %染料及其中間體等有機物與1 4 · 9 5 %氯化鈉。於常 壓、1 0 3〜1 0 7 °C條件下進行蒸發結晶,餾出i 3 〇 0m丨冷凝 液’冷凝液pH值為3.29,内含65.5ppm氣化鈉,另殘留約 7 0 0 m 1含氣化鈉晶體的懸浮液。經過濾得表面帶紫色的濕 氯化鈉晶體,添加3 0 〇 m 1飽和鹽液,於4 5〜5 0 °C、陰陽極' 位差為4V的條件下進行電解氧化,3〇分鐘後溶液成為备電 透明,經過濾、乾燥得1 3 0 g純度為9 9 · 4 3 %的白色氣化色· 體。 '納晶Page 574059 V. Description of the invention (6) Liquid 'electrolytic oxidation under the conditions of 4 5 ~ 5 C_ and the potential difference between cathode and anode is 5 v' 3 After 10 minutes, the Luo liquid became colorless and transparent, and was filtered and dried to obtain 2 3 5 g of white sodium vapor crystals with a purity of 99.57% were higher than A cs reagent grade standard 99.5 ° / 〇. Example 3 3,000 ml of a concentrated violet-blue dye was used to salt out the waste liquid. The pH value of the waste liquid was 8.91, which contained 1.64% dye. Its intermediates and other organic matter and 6.00% sodium chloride. Evaporate and crystallize at 80torr, 60 ~ 65 ° C. 2000ml of condensate is distilled off. The condensate has a pH of 7.85, contains 6.5 ppm sodium chloride, and about 100% remains. 0 m 1 suspension containing vaporized nanocrystals. After filtering, a purple-blue wet emulsified nanobody was added, and a saturated salt solution of 3 〇η 1 was added. The electrolytic oxidation was performed at a temperature of 4 ° to 4 5 ° C and a potential difference between anode and anode of 4 V. After 60 minutes, The solution became colorless and transparent, and was filtered and dried to obtain 220 g of white sodium chloride crystals with a purity of 99.52%. Example 4 2000 ml of concentrated purple dye was used to salt out the waste liquid. The pH value of the waste liquid was 4.78, which contained 1.34% organic matter such as dyes and intermediates, and 14.95% sodium chloride. Evaporate and crystallize at atmospheric pressure at 10 3 ~ 107 ° C, distill off i 3 0 0 0 m 丨 Condensate 'Condensate pH is 3.29, contains 65.5 ppm sodium gasification, and about 7 0 0 m 1 suspension containing vaporized sodium crystals. After filtering to obtain purple wet sodium chloride crystals on the surface, 300 m 1 of saturated saline solution was added, and electrolytic oxidation was performed at a temperature of 4 5 to 50 ° C and a cathode-anode difference of 4V. The solution became transparent, and was filtered and dried to obtain 130 g of a white gaseous color and a body with a purity of 99.43%. 'Nanocrystalline
574059 五、發明說明(7) 藉由上述實施例,明顯了解本發明技術可在常壓、低 溫的條件下,輕易由染料鹽析廢液回收製得高純度氯化鈉 或氯化鉀晶體,而無習用技術之缺點,確實具有相當之高 進步性,利於產業上的應用,惟依法提出發明專利申請, 祈 貴審查委員早曰准予專利為禱。 雖本發明以較佳實施例揭露如上,但並非用以限定本發明 實施之範圍;任何熟習此項技藝者,在不脫離本發明之精 神和範圍内,當可作些許之更動與潤飾,即凡依本發明所 做的均等變化與修飾,應為本發明專利範圍所涵蓋,其界 定應以申請專利範圍為準,合先陳明。574059 V. Description of the invention (7) Through the above examples, it is clearly understood that the technology of the present invention can easily recover high-purity sodium chloride or potassium chloride crystals from dye salting-out waste liquid under normal pressure and low temperature conditions. The disadvantages of non-conventional technology are indeed quite advanced, which is conducive to industrial applications. However, the invention patent application is filed in accordance with the law. It is hoped that the examiner would grant the patent earlier. Although the present invention is disclosed as above with a preferred embodiment, it is not intended to limit the scope of implementation of the present invention. Any person skilled in the art can make some changes and decorations without departing from the spirit and scope of the present invention, that is, All equal changes and modifications made in accordance with the present invention shall be covered by the patent scope of the present invention, and the definition shall be based on the scope of the patent application, and shall be declared together.
第10頁 574059 圖式簡單說明 第一圖係為本發明之處理流程圖 圖號簡單說明: 1 · · · ·染料鹽析廢液 2 3 4 5 6 7 8 9 0Page 10 574059 Brief description of the diagram The first diagram is the process flow chart of the present invention. Brief description of the diagram number: 1 · · · · Dye salting out waste liquid 2 3 4 5 6 7 8 9 0
1617 18 19 2 0 2 1 中和 蒸發結晶 冷凝液 有機懸浮物 次級染料 焚化 懸浮液 過濾 濾、液 回流 濕晶體 新鮮鹽液或回收鹽液 懸浮液 電解氧化 過濾、 濾液 回流 濕晶體 乾燥 高純度氣化鈉或氯化鉀晶體 «1617 18 19 2 0 2 1 Neutralization evaporation crystallization condensate organic suspension secondary dye incineration suspension filtration filtration, liquid reflux wet crystal fresh salt solution or recovery salt suspension electrolytic oxidation filtration, filtrate reflux wet crystal drying high purity gas Sodium or potassium chloride crystals «
第11頁Page 11
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106946396A (en) * | 2017-05-12 | 2017-07-14 | 江苏汇方环境科技有限公司 | A kind of integrated treatment technology of wastewater of chemical industry with high concentration recycling |
CN107982941A (en) * | 2017-11-14 | 2018-05-04 | 天津大学 | The control method of sodium-chloride water solution intermittent vacuum evaporative mass |
US10364162B2 (en) | 2017-06-30 | 2019-07-30 | National Tsing Hua University | System and method for treating salt-containing glycerin wastewater |
-
2001
- 2001-09-21 TW TW90123323A patent/TW574059B/en active
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106946396A (en) * | 2017-05-12 | 2017-07-14 | 江苏汇方环境科技有限公司 | A kind of integrated treatment technology of wastewater of chemical industry with high concentration recycling |
US10364162B2 (en) | 2017-06-30 | 2019-07-30 | National Tsing Hua University | System and method for treating salt-containing glycerin wastewater |
CN107982941A (en) * | 2017-11-14 | 2018-05-04 | 天津大学 | The control method of sodium-chloride water solution intermittent vacuum evaporative mass |
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