[go: up one dir, main page]

TWI645045B - A seperation method of cerium oxide abrasive and glass powder - Google Patents

A seperation method of cerium oxide abrasive and glass powder Download PDF

Info

Publication number
TWI645045B
TWI645045B TW106132781A TW106132781A TWI645045B TW I645045 B TWI645045 B TW I645045B TW 106132781 A TW106132781 A TW 106132781A TW 106132781 A TW106132781 A TW 106132781A TW I645045 B TWI645045 B TW I645045B
Authority
TW
Taiwan
Prior art keywords
powder
cerium oxide
organic solvent
oxide polishing
glass powder
Prior art date
Application number
TW106132781A
Other languages
Chinese (zh)
Other versions
TW201915176A (en
Inventor
王立邦
卓昀蓁
江育華
張添晉
Original Assignee
國立臺北科技大學
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 國立臺北科技大學 filed Critical 國立臺北科技大學
Priority to TW106132781A priority Critical patent/TWI645045B/en
Application granted granted Critical
Publication of TWI645045B publication Critical patent/TWI645045B/en
Publication of TW201915176A publication Critical patent/TW201915176A/en

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Landscapes

  • Grinding-Machine Dressing And Accessory Apparatuses (AREA)

Abstract

本發明係一種氧化鈰拋光粉與玻璃粉的分離方法,係直接分離粉末混合物中的氧化鈰拋光粉及玻璃粉,包括前處理、分散處理、調整酸鹼值處理、添加捕集劑處理、混合處理、靜置處理、離心處理、烘乾處理。尤其是,在混合處理時加入有機溶劑,進而產生互不相溶且上下分離的有機溶劑相及水相,並在適當的酸鹼下,利用捕集劑改變表面活性,使得氧化鈰拋光粉或玻璃粉富含於有機溶劑相或水相中,藉以達到分離功效。因此,本發明不會產生二次污染性廢水,且消耗能源較少,不需特別裝置,因而整體的操作、維護簡單。The invention relates to a method for separating cerium oxide polishing powder and glass powder, which directly separates the cerium oxide polishing powder and the glass powder in the powder mixture, including pretreatment, dispersion treatment, adjustment of pH value treatment, addition of collector treatment, mixing Treatment, static treatment, centrifugal treatment, and drying treatment. In particular, an organic solvent is added during the mixing treatment to produce an organic solvent phase and an aqueous phase which are incompatible with each other and separated from each other, and the surfactant is used to change the surface activity under a suitable acid and alkali to make the cerium oxide polishing powder or The glass powder is enriched in an organic solvent phase or an aqueous phase to achieve separation efficiency. Therefore, the present invention does not generate secondary polluted wastewater, and consumes less energy, and does not require special equipment, so that the overall operation and maintenance are simple.

Description

氧化鈰拋光粉與玻璃粉的分離方法Method for separating cerium oxide polishing powder and glass powder

本發明係有關於一種氧化鈰拋光粉與玻璃粉的分離方法,尤其是利用去離子水、有機溶劑以製造水相及有機溶劑相,並添加酸鹼值調整劑以獲得最佳酸鹼值,再藉表面活性劑的界面特性加強分離功效,因而改善氧化鈰拋光粉、玻璃粉在整體水相及有機溶劑相中的穩定性及分離回收效率,同時可避免產生二次污染廢水的問題。The invention relates to a method for separating a cerium oxide polishing powder and a glass powder, in particular, using deionized water, an organic solvent to produce an aqueous phase and an organic solvent phase, and adding a pH adjusting agent to obtain an optimum pH value. The interface property of the surfactant enhances the separation efficiency, thereby improving the stability and separation and recovery efficiency of the cerium oxide polishing powder, the glass powder in the whole aqueous phase and the organic solvent phase, and avoiding the problem of secondary pollution of the wastewater.

目前,稀土金屬已廣泛應用在許多電子、機械、航太工業上,其中鈰(Ce)可做為氧化劑、拋光粉、玻璃和瓷器的黃色染料、石油提煉液體催化過程(FCC)催化劑,因而更加引起業界對於回收,再利用技術的注意。At present, rare earth metals have been widely used in many electronic, mechanical, and aerospace industries. Among them, cerium (Ce) can be used as an oxidant, polishing powder, yellow dye for glass and porcelain, and petroleum refining liquid catalytic process (FCC) catalyst. Caused the industry to pay attention to recycling and reuse technology.

進一步仔細分析,由於鈰能吸收紫外線與紅外線,現已被大量應用於汽車玻璃,比如當作玻璃添加劑,不僅能防紫外線,還可降低車內溫度,從而節約空調用電。再者,汽車尾氣淨化催化劑也使用鈰,可有效防止大量汽車廢氣排到空氣中。在顏料、塗料、油墨和紙張方面,硫化鈰可以取代鉛、鎘等對環境和人類有害的金屬,不僅可對塑料著色,還可用於塗料、油墨和紙張等行業。此外,在先進的固體激光器上,美國已研製出Ce:LiSAF激光系統固體激光器,如果通過監測色氨酸濃度,還可用於探查生物武器,或應用於醫學方面。Further careful analysis, because 铈 can absorb ultraviolet and infrared rays, has been widely used in automotive glass, for example, as a glass additive, not only can prevent ultraviolet rays, but also reduce the temperature inside the car, thereby saving air conditioning electricity. In addition, car exhaust purification catalysts also use helium, which can effectively prevent a large amount of automobile exhaust gas from being discharged into the air. In pigments, coatings, inks and papers, barium sulfide can replace metals that are harmful to the environment and humans, such as lead and cadmium. It can be used not only for coloring plastics, but also for coatings, inks and paper. In addition, on advanced solid-state lasers, the Ce:LiSAF laser system solid-state laser has been developed in the United States. It can also be used to probe biological weapons or in medical applications by monitoring the concentration of tryptophan.

另外,鈰也被應用在鏡頭、三稜鏡等光學玻璃的拋光研磨處理所使用的氧化鈰系拋光粉。一般,氧化鈰系拋光粉係將Monazite (獨居石、磷鈰鑭礦)等含有以鈰為主之稀土金屬化合物的礦物,經由燒結、粉碎等加工處理後製造而成。由於氧化鈰具有可以和玻璃的主要成分元素-二氧化矽的化學反應性,因而被用來作為精密研磨時所使用的化學機械研磨(Chemical Mechanical Polishing,CMP)的拋光粉原料使用。In addition, bismuth is also used in the cerium oxide-based polishing powder used for polishing and polishing of optical glass such as lenses and lenses. In general, the cerium oxide-based polishing powder is produced by processing a mineral containing a rare earth metal compound such as Monazite (monistry, xenotime) and the like by sintering or pulverization. Since cerium oxide has chemical reactivity with cerium oxide, a main component of glass, it is used as a polishing powder raw material for chemical mechanical polishing (CMP) used in precision polishing.

近年來,隨著電子資訊產業的快速成長,光罩、平板顯示器等平面透明玻璃的使用量增加,氧化鈰系拋光粉的需求亦隨之增加。In recent years, with the rapid growth of the electronic information industry, the use of flat transparent glass such as photomasks and flat panel displays has increased, and the demand for cerium oxide-based polishing powder has also increased.

目前,在面板玻璃、光學鏡片等玻璃的生產製造過程中,主要是將氧化鈰系拋光粉於水中分散成拋光液後,供玻璃拋光研磨使用,以去除經蝕刻減薄處理後所產生的微細紋痕。不過,研磨後產生的拋光廢液中,即含有以氧化鈰等稀土金屬為主的氧化鈰系拋光粉及玻璃碎屑粉的微粒子混合物,而且在使用一段時間後,會因拋光粉的劣化以及玻璃碎屑粉混入拋光粉中,而無法維持原有的拋光研磨速度,或造成玻璃表面的損傷,甚至廢棄,因而產生大量的氧化鈰玻璃拋光廢棄物。一般最簡單的處理方式是直接進行掩埋處理,並未進行有效的分離回收,導致稀土金屬資源的浪費。At present, in the production process of glass such as panel glass and optical lens, the cerium oxide-based polishing powder is mainly dispersed into water into a polishing liquid, and then used for polishing and polishing the glass to remove fine particles generated by etching and thinning treatment. Smudges. However, the polishing waste liquid produced after the grinding contains a fine particle mixture of cerium oxide-based polishing powder and glass crumb powder mainly composed of a rare earth metal such as cerium oxide, and may be deteriorated by the polishing powder after being used for a while. The glass crumb powder is mixed into the polishing powder, and the original polishing and polishing speed cannot be maintained, or the glass surface is damaged or even discarded, thereby generating a large amount of cerium oxide glass polishing waste. Generally, the simplest processing method is to directly perform the buried treatment, and the effective separation and recovery are not performed, resulting in waste of rare earth metal resources.

為解決上述問題,習用技術的回收方法包括強酸氧化熱處理法、強酸-雙氧水浸漬法、氯化揮發法、強鹼浸漬法、泡沫浮選法及熱處理、強鹼法加氟化鈉、混凝法等等。雖然這類方法可從氧化鈰玻璃拋光廢棄物中回收稀土金屬,不過卻也存在著必須使用大量強酸、強鹼等化學藥品,處理成本昂貴,而且還在進行高溫處理時消耗大量能源,並在回收過程中產生二次污染廢水。In order to solve the above problems, conventional techniques for recovery include strong acid oxidation heat treatment, strong acid-hydrogen peroxide impregnation, chlorination volatilization, strong alkali impregnation, froth flotation and heat treatment, strong alkali method plus sodium fluoride, and coagulation and many more. Although this type of method can recover rare earth metals from bismuth oxide glass polishing waste, there are also a large number of chemicals such as strong acids and alkalis, which are expensive to process and consume a lot of energy during high temperature processing. Secondary pollution wastewater is generated during the recovery process.

具體而言,在強酸氧化熱處理中,是先以草酸去除凝聚劑,再使用氫氧化鈉溶液溶解玻璃粉,經1450 mesh過篩後,以90℃乾燥2小時,並透過高溫600℃焙燒2小時後,加入6N硫酸,再加入Na 2SO 4而在50℃下,反應4小時以去除鈰以外的稀土元素,接著通過選擇性沉澱,使得鈰的純度增加至94%,同時完全除去鑭。使用硫酸鈉沉澱稀土鹽的最佳條件是入Na 2SO 4/ RE = 0.5,並得知產率約為60%。 Specifically, in the strong acid oxidation heat treatment, the coagulant is first removed with oxalic acid, and the glass frit is dissolved by using a sodium hydroxide solution, sieved through a 1450 mesh, dried at 90 ° C for 2 hours, and fired at a high temperature of 600 ° C for 2 hours. Thereafter, 6N sulfuric acid was added, and Na 2 SO 4 was further added thereto to carry out a reaction at 50 ° C for 4 hours to remove rare earth elements other than cerium, followed by selective precipitation to increase the purity of cerium to 94% while completely removing cerium. The optimum conditions for the precipitation of the rare earth salt using sodium sulfate are Na 2 SO 4 / RE = 0.5, and the yield is about 60%.

強酸-雙氧水浸漬法是利用HNO 3/H 2O 2混合物以溶解氧化鈰系拋光廢棄物,並將氧化鈰等稀土金屬以碳酸鹽化合物的形式沉澱,隨後利用高溫焙燒將稀土金屬由碳酸鹽轉變的氧化物。此方法可以從1 kg的拋光廢棄物中,產生0.8 kg的新拋光粉。 The strong acid-hydrogen peroxide impregnation method utilizes a mixture of HNO 3 /H 2 O 2 to dissolve the cerium oxide polishing waste, and precipitates a rare earth metal such as cerium oxide as a carbonate compound, and then converts the rare earth metal from carbonate by high temperature baking. Oxide. This method produces 0.8 kg of new polishing powder from 1 kg of polishing waste.

氯化揮發法是利用氯氣/氮氣的混合氣體,將氧化鈰系玻璃拋光廢棄物中的氧化鈰等稀土金屬,於高溫之下進行氯化及揮發反應。利用稀土金屬的氯化物揮發溫度(800-900℃),與其他金屬的氯化物揮發溫度的差異。例如,鈷或鎳的氯化物 500-700℃、鐵銅鋁的氯化物350℃以下)而進行分離,在過程中獲得最高品位約80%的LaCl 3和CeCl 3The chlorination volatilization method is a chlorination and volatilization reaction of a rare earth metal such as cerium oxide in a cerium oxide-based glass polishing waste by using a mixed gas of chlorine gas/nitrogen gas. The difference between the chloride volatilization temperature of the rare earth metal (800-900 ° C) and the chloride volatilization temperature of other metals. For example, cobalt or nickel chloride is 500-700 ° C, iron-copper-aluminum chloride is below 350 ° C), and the highest grade is about 80% of LaCl 3 and CeCl 3 .

濕法冶金法是用以將稀土元素(REE)和大量稀土氧化物之稀土拋光廢棄物(REPPWs)中分離,其主要成分為氧化鈰,其次為氧化鑭、氧化鐠和氧化釹,而所採用的技術手段包含五個部分:第一部分,利用NaSO 4-H 2SO 4-H 2O在95-125℃下 對REPPWs反應形成NaRE(SO 4) 2∙H 2O;第二部分,添加NaOH將NaRE(SO 4) 2∙H 2O形成RE(OH) 3;第三部分,利用O 2將Ce(OH) 3氧化為Ce(OH) 4,其有利於將REPPWs中主要相存在的鈰與其它REE分離;第四部分,利用HCl於25℃下酸浸洗至pH 2.5到3.5間,其浸出後可獲得Ce以外高產率之REE;第五部分,將殘餘物添加H 2SO 4以分離Ce。 The hydrometallurgy method is used to separate rare earth elements (REE) and rare earth oxides from rare earth polishing wastes (REPPWs). The main component is cerium oxide, followed by cerium oxide, cerium oxide and cerium oxide. The technical means consists of five parts: the first part, using NaSO 4 -H 2 SO 4 -H 2 O to react with REPPWs at 95-125 ° C to form NaRE(SO 4 ) 2 ∙H 2 O; the second part, adding NaOH NaRE(SO 4 ) 2 ∙H 2 O forms RE(OH) 3 ; the third part, O 2 is used to oxidize Ce(OH) 3 to Ce(OH) 4 , which is beneficial to the presence of ruthenium in the main phase of REPPWs Separated from other REE; the fourth part, acid leaching with HCl at 25 ° C to pH between 2.5 and 3.5, after leaching, a high yield of REE other than Ce can be obtained; in the fifth part, the residue is added with H 2 SO 4 Separate Ce.

然而,上述習用技術的缺點在於皆須使用大量昂貴化學藥品,以及消耗大量能源的高溫處理,尤其是在回收過程中還會產生二次污染廢水。However, the above-mentioned conventional techniques have disadvantages in that a large amount of expensive chemicals and high-temperature treatments that consume a large amount of energy are required, and particularly, secondary pollution wastewater is generated in the recycling process.

因此,非常需要一種創新的氧化鈰拋光粉與玻璃粉的分離方法,可對氧化鈰拋光粉與玻璃碎屑粉的混合粉體進行直接分離而回收氧化鈰拋光粉,不但可促進氧化鈰拋光粉的循環再利用,還能做為各種稀土金屬的二次資源使用,藉以解決上述習用技術的所有問題。Therefore, there is a great need for an innovative separation method of cerium oxide polishing powder and glass powder, which can directly separate the mixed powder of cerium oxide polishing powder and glass crumb powder to recover cerium oxide polishing powder, which can promote cerium oxide polishing powder. Recycling can also be used as a secondary resource for various rare earth metals to solve all the problems of the above-mentioned conventional technologies.

本發明之主要目的在於提供一種氧化鈰拋光粉與玻璃粉的分離方法,係用以將粉末混合物中的氧化鈰拋光粉及玻璃粉,藉分離、回收而再利用,主要包括以下依序進行的處理步驟。The main object of the present invention is to provide a method for separating cerium oxide polishing powder and glass powder, which is used for separating and recycling cerium oxide polishing powder and glass powder in a powder mixture, mainly including the following steps. Processing steps.

首先進行前處理,加入去離子水於包含氧化鈰拋光粉及玻璃粉的原始混合物中,並混合成粉末混合漿料。氧化鈰拋光粉及玻璃粉在原始混合物的重量比例分別為100:1至1:1之間。接著,執行分散處理,利用超音波分散機分散粉末混合漿料的氧化鈰拋光粉及玻璃粉,且分散處理是進行二分鐘至二小時之間。First, pretreatment is carried out, and deionized water is added to the original mixture containing the cerium oxide polishing powder and the glass powder, and mixed into a powder mixed slurry. The weight ratio of the cerium oxide polishing powder and the glass powder in the original mixture is between 100:1 and 1:1, respectively. Next, dispersion treatment is performed, and the cerium oxide polishing powder and the glass powder of the powder mixed slurry are dispersed by an ultrasonic disperser, and the dispersion treatment is performed for two minutes to two hours.

然後,在調整酸鹼值處理中加入酸性調整劑或鹼性調整劑的酸鹼值調整劑,以調整粉末混合漿料的酸鹼值至目標酸鹼值,比如目標酸鹼值可為pH4至pH10之間。進行添加捕集劑處理,添加捕集劑以當作界面活性劑,用以對粉末混合漿料所包含的氧化鈰拋光粉或玻璃粉產生捕集作用,其中捕集劑可為陰離子捕集劑或陽離子捕集劑,且捕集劑的濃度可為0.5 kg/ton至10.0 kg/ton之間。Then, adding a pH adjuster or a pH adjuster to adjust the pH value of the powder mixed slurry to a target pH value, for example, the target pH value may be pH 4 to Between pH10. Adding a collector treatment, adding a collector as a surfactant to capture a cerium oxide polishing powder or a glass powder contained in the powder mixed slurry, wherein the collector may be an anion collector Or a cationic collector, and the concentration of the collector can be between 0.5 kg/ton and 10.0 kg/ton.

之後,在混合處理中利用搖盪機所產生的搖盪力,對粉末混合漿料進行初階混合,操作時間為二分鐘至二小時之間,隨後再添加有機溶劑,其中有機溶劑是不互溶於去離子水,且有機溶劑對該去離子水的重量比為100:1至1:1之間,同時利用搖盪機進行進階混合而形成粉末混合液,且進階混合的操作時間為二分鐘至二小時之間。Then, in the mixing process, the powder mixed slurry is subjected to preliminary mixing by using the shaking force generated by the oscillating machine, and the operation time is between two minutes and two hours, and then an organic solvent is added, wherein the organic solvent is not mutually soluble. Ionic water, and the weight ratio of the organic solvent to the deionized water is between 100:1 and 1:1, and the powder mixture is formed by advanced mixing using a shaker, and the operation time of the advanced mixing is two minutes to Between two hours.

粉末混合液經靜置處理約至少二十分鐘,形成上下相互分離的有機溶劑相溶液及水相溶液,再分別取出有機溶劑相溶液及水相溶液,其中有機溶劑相溶液及水相溶液可分別富含氧化鈰拋光粉或富含該玻璃粉。再進行離心處理,有機溶劑相溶液及水相溶液是分別利用相對應的離心機所產生的離心力以分離其中的固體物及液體,並取出固體物,其中有機溶劑相溶液的固體物或水相的固體物係包含氧化鈰拋光粉或玻璃粉。The powder mixture is allowed to stand for at least twenty minutes to form an organic solvent phase solution and an aqueous phase solution separated from each other, and then the organic solvent phase solution and the aqueous phase solution are respectively taken out, wherein the organic solvent phase solution and the aqueous phase solution are respectively respectively Rich in cerium oxide polishing powder or rich in the glass powder. After centrifugation, the organic solvent phase solution and the aqueous phase solution are respectively separated by the centrifugal force generated by the corresponding centrifuge to separate the solid matter and the liquid therein, and the solid matter is taken out, wherein the organic solvent phase solution is solid or water phase. The solid system contains cerium oxide polishing powder or glass powder.

最後進行烘乾處理,利用烘乾機加熱由有機溶劑相溶液中所取出的固體物或由水相中所取出的固體物,藉以蒸發、去除殘留的液體,進而分別得到氧化鈰拋光粉或玻璃粉,達到回收的目的。Finally, the drying process is performed, and the solid matter taken out from the organic solvent phase solution or the solid matter taken out from the aqueous phase is heated by a dryer to evaporate and remove the residual liquid, thereby respectively obtaining cerium oxide polishing powder or glass. Powder, to achieve the purpose of recycling.

因此,本發明可在不產生二次污染性廢水下,利用可相互分離的有機溶劑相以及水相而直接、有效分離原始混合物中的氧化鈰拋光粉及玻璃粉,不只所消耗的能源較少,因且還能大幅提升整體的分離效應。此外,本發明不需配置特別裝置,即能藉一般分離設備而實施,因而操作成本低,且整體的操作、維護簡單。Therefore, the present invention can directly and effectively separate the cerium oxide polishing powder and the glass powder in the original mixture by using the mutually separable organic solvent phase and the water phase without generating secondary pollution wastewater, and not only consume less energy. Because it can also greatly improve the overall separation effect. In addition, the present invention does not need to be configured with a special device, that is, can be implemented by a general separation device, so that the operation cost is low, and the overall operation and maintenance are simple.

以下配合圖示及元件符號對本發明之實施方式做更詳細的說明,俾使熟習該項技藝者在研讀本說明書後能據以實施。The embodiments of the present invention will be described in more detail below with reference to the drawings and the reference numerals, which can be implemented by those skilled in the art after having studied this specification.

參考第一圖,本發明實施例氧化鈰拋光粉與玻璃粉的分離方法的示意圖。如第一圖所示,本發明氧化鈰拋光粉與玻璃粉的分離方法包括依序進行的步驟S10、S20、S30、S40、S50、S60、S70以及S80,分別為前處理、分散處理、調整酸鹼值處理、添加捕集劑處理、混合處理、靜置處理、離心處理、烘乾處理,用以將原始粉末混合物中的氧化鈰(CeO 2)拋光粉及玻璃粉,藉分離、回收而再利用。 Referring to the first figure, a schematic diagram of a method for separating cerium oxide polishing powder and glass powder according to an embodiment of the present invention. As shown in the first figure, the method for separating the cerium oxide polishing powder and the glass powder of the present invention comprises the steps S10, S20, S30, S40, S50, S60, S70 and S80 which are sequentially performed, respectively, pre-processing, dispersion processing, and adjustment. The pH treatment, the addition of the collector treatment, the mixing treatment, the static treatment, the centrifugation treatment, and the drying treatment are used to separate and recover the cerium oxide (CeO 2 ) polishing powder and the glass powder in the original powder mixture. Reuse.

同時還可參考第二圖,藉以初步了解本發明分離方法所要達成的功效,其中第二圖的左側顯示原始粉末混合物中的玻璃粉G是沾附於氧化鈰拋光粉P的表面,因為玻璃粉G一般是小於氧化鈰拋光粉P,而第二圖的中間顯示經分散處理後,玻璃粉G及氧化鈰拋光粉P已大致上相互分散、分開,且第二圖的右側是顯示玻璃粉G及氧化鈰拋光粉P最後經本發明的靜置處理、離心處理、烘乾處理後已完成分離而回收。At the same time, reference may also be made to the second figure for a preliminary understanding of the efficacy to be achieved by the separation method of the present invention, wherein the left side of the second figure shows that the glass powder G in the original powder mixture is adhered to the surface of the cerium oxide polishing powder P because the glass powder G is generally smaller than the cerium oxide polishing powder P, and the middle portion of the second figure shows that after the dispersion treatment, the glass powder G and the cerium oxide polishing powder P have been substantially dispersed and separated from each other, and the right side of the second figure shows the glass powder G. And the cerium oxide polishing powder P is finally recovered by the static treatment, the centrifugal treatment, and the drying treatment of the present invention.

首先,在步驟S10中進行前處理,包括將適當量的去離子水加入到包含氧化鈰拋光粉及玻璃粉的原始混合物中,並混合成粉末混合漿料,其中氧化鈰拋光粉及玻璃粉在原始混合物的重量比例分別為100:1至1:1之間,再者原始混合物具有0.2 μm至~60.5 μm的粒徑範圍,且平均粒徑(D 50)為1.8 μm至3.5 μm。 First, the pretreatment is performed in step S10, comprising adding an appropriate amount of deionized water to the original mixture containing the cerium oxide polishing powder and the glass powder, and mixing into a powder mixed slurry, wherein the cerium oxide polishing powder and the glass powder are The original mixture has a weight ratio of between 100:1 and 1:1, and the original mixture has a particle size range of 0.2 μm to ~60.5 μm and an average particle diameter (D 50 ) of 1.8 μm to 3.5 μm.

由於原始混合物可能會含有不純物、分散劑或潤滑液等物質而導致實際樣品的表面性質有所變化,所以為了避免影響整體的分離回收效果,可在前處理中,額外包括過濾處理或去油處理,藉以分別去除顆粒狀不純物質或油狀潤滑液,並可針對分散劑的特性進行相對應的有效分離處理。Since the original mixture may contain substances such as impurities, dispersants or lubricating fluids, which may cause changes in the surface properties of the actual sample, in order to avoid affecting the overall separation and recovery effect, it may additionally include filtration treatment or degreasing treatment in the pretreatment. In order to remove particulate impure substances or oily lubricating fluids separately, and corresponding effective separation treatment for the characteristics of the dispersing agents.

接著,進行步驟S20的分散處理,主要是利用超音波分散機,分散粉末混合漿料中相互貼附的氧化鈰拋光粉及玻璃粉,其中整個分散處理的操作是進行二分鐘至二小時。Next, the dispersion treatment in the step S20 is carried out, mainly by dispersing the cerium oxide polishing powder and the glass powder adhered to each other in the powder mixed slurry by means of an ultrasonic disperser, wherein the entire dispersion treatment is carried out for two minutes to two hours.

在步驟S30中進行調整酸鹼值處理,係加入酸鹼值調整劑以調整粉末混合漿料的酸鹼值至目標酸鹼值,其中酸鹼值調整劑可為酸性調整劑或鹼性調整劑。舉例而言,酸性調整劑可選用鹽酸及硝酸的至少其中之一,而鹼性調整劑可選用氫氧化鈉及氫氧化鉀的至少其中之一。此外,目標酸鹼值可為pH4至pH10之間。Adjusting the pH value in step S30, adding a pH adjuster to adjust the pH value of the powder mixed slurry to a target pH value, wherein the pH adjuster may be an acid regulator or an alkali regulator . For example, the acid regulator may be at least one of hydrochloric acid and nitric acid, and the alkaline regulator may be at least one of sodium hydroxide and potassium hydroxide. In addition, the target pH value can be between pH 4 and pH 10.

然後進入步驟S40執行添加捕集劑處理,係添加捕集劑以當作界面活性劑,其中捕集劑可為陰離子捕集劑或陽離子捕集劑,用以對粉末混合漿料所包含的氧化鈰拋光粉或玻璃粉產生捕集作用。捕集劑在有機溶劑的濃度可為0.5 kg/ton至10.0 kg/ton之間。例如,捕集劑包含十二烷基硫酸鈉(Sodium Dodecyl Sulfate,SDS)、油酸鈉(Sodium Oleate,NaOL)及十二烷胺醋酸鹽(Dodecylamine Acetate,DAA )的其中之一。要注意的是,步驟S30中的目標酸鹼值必須配合步驟S40所使用的捕集劑,藉以提升整體效率,比如,在使用SDS時,目標酸鹼值為pH8.0至pH9.5之間,在使用NaOL時,目標酸鹼值為pH7或pH7至pH7.5之間,在使用DAA時,目標酸鹼值為pH8.0至pH9.5之間。Then, proceeding to step S40, an additive collector treatment is performed, and a collector is added to act as a surfactant, wherein the collector may be an anion collector or a cationic collector for oxidizing the powder mixed slurry.铈 Polishing powder or glass powder produces a trapping effect. The concentration of the collector in the organic solvent can range from 0.5 kg/ton to 10.0 kg/ton. For example, the collector comprises one of Sodium Dodecyl Sulfate (SDS), Sodium Oleate (NaOL), and Dodecylamine Acetate (DAA). It should be noted that the target pH value in step S30 must match the collector used in step S40 to improve the overall efficiency. For example, when using SDS, the target pH value is between pH 8.0 and pH 9.5. When NaOL is used, the target pH value is between pH 7 or pH 7 to pH 7.5, and when DAA is used, the target pH value is between pH 8.0 and pH 9.5.

進入步驟S50執行混合處理,主要是利用搖盪機,藉所產生的搖盪力而對粉末混合漿料進行初階混合,且初階混合的操作係維持二分鐘至二小時之間,之後,再添加定的有機溶劑,且有機溶劑是不互溶於去離子水,並再次利用搖盪機進行進階混合而形成混合均勻的粉末混合液,且進階混合的操作係維持二分鐘至二小時之間。尤其,有機溶劑對去離子水的重量比可為100:1至1:1之間,而且有機溶劑是包含異辛烷(isooctane)、十二烷(dodecane)或煤油(kerosine)。Proceeding to step S50, the mixing process is performed, mainly by using a swinging machine, and the powder mixing slurry is subjected to preliminary mixing by the generated shaking force, and the operation of the preliminary mixing is maintained for two minutes to two hours, and then added. The organic solvent is fixed, and the organic solvent is not mutually soluble in deionized water, and is further mixed by a shaker to form a uniformly mixed powder mixture, and the operation of the advanced mixing is maintained for two minutes to two hours. In particular, the weight ratio of organic solvent to deionized water may be between 100:1 and 1:1, and the organic solvent comprises isooctane, dodecane or kerosine.

之後,進行步驟S60的靜置處理,將粉末混合液靜置至少二十分鐘,形成上下相互分離的有機溶劑相溶液及水相溶液,其中有機溶劑相溶液因比重作用,一般是在水相溶液的上方。同時,分別取出有機溶劑相溶液及水相溶液,比如利用一般的分液漏斗而分離、取出。要注意的是,使用SDS及NaOL為捕集劑時,有機溶劑相溶液富含氧化鈰拋光粉,而水相溶液富含玻璃粉。使用DAA為捕集劑時,有機溶劑相溶液富含玻璃粉,而水相溶液富含氧化鈰拋光粉。Thereafter, the static treatment in step S60 is performed, and the powder mixture is allowed to stand for at least twenty minutes to form an organic solvent phase solution and an aqueous phase solution separated from each other, wherein the organic solvent phase solution is generally in the aqueous phase solution due to specific gravity. Above. At the same time, the organic solvent phase solution and the aqueous phase solution are separately taken out, for example, separated and taken out using a general separatory funnel. It should be noted that when SDS and NaOL are used as the collector, the organic solvent phase solution is rich in cerium oxide polishing powder, and the aqueous phase solution is rich in glass powder. When DAA is used as a collector, the organic solvent phase solution is rich in glass frit, and the aqueous phase solution is rich in cerium oxide polishing powder.

在步驟S70中,進行離心處理,主要是對步驟S60中所得的有機溶劑相溶液及水相溶液分別利用相對應的離心機,藉所產生的離心力而產生固液分離作用,進而分離並取出其中位於底部的固體物以及位於上部的澄清之液體。具體而言,使用SDS及NaOL為捕集劑時,有機溶劑相溶液的固體物主要包含氧化鈰拋光粉,且水相溶液的固體物主要包含玻璃粉。使用DAA為捕集劑時,有機溶劑相溶液富含玻璃粉,而水相溶液富含氧化鈰拋光粉。In step S70, the centrifugation process is performed, mainly, the organic solvent phase solution and the aqueous phase solution obtained in step S60 are respectively subjected to solid-liquid separation by the centrifugal force generated by using the corresponding centrifuge, and then separated and taken out. The solid at the bottom and the clarified liquid at the top. Specifically, when SDS and NaOL are used as the collector, the solid matter of the organic solvent phase solution mainly contains cerium oxide polishing powder, and the solid matter of the aqueous phase solution mainly contains glass frit. When DAA is used as a collector, the organic solvent phase solution is rich in glass frit, and the aqueous phase solution is rich in cerium oxide polishing powder.

最後進入步驟S80中以執行烘乾處理,係利用烘乾機對對步驟S70中所得的固體物進行加熱,藉以蒸發並去除掉殘留的液體,進而獲得氧化鈰拋光粉及玻璃粉,達到回收的目的。Finally, the process proceeds to step S80 to perform the drying process, and the solid matter obtained in step S70 is heated by the dryer to evaporate and remove the residual liquid, thereby obtaining cerium oxide polishing powder and glass powder to achieve recovery. purpose.

為進一步說明本發明所達成功效,以下將列舉示範性的實例。To further illustrate the efficacy achieved by the present invention, exemplary examples are listed below.

首先,有機溶劑是使用異辛烷,並以SDS當作捕集劑,而且氧化鈰拋光粉與玻璃粉的混合重量比例為1:1,其結果顯示第三A圖及第三B圖。First, the organic solvent was isooctane and SDS was used as a collector, and the mixing ratio of the cerium oxide polishing powder to the glass powder was 1:1, and the results showed a third A chart and a third B chart.

在添加1 kg/ton及2.5 kg/ton的SDS下,在各pH下的異辛烷相回收物中氧化鈰拋光粉與水相回收物中玻璃粉的品位及回收率,是隨著pH值的增加而上升,並於大約pH 9時,添加2.5 kg/ton SDS時具有最佳的品位為86.8%,其回收率為91.7%,不過,在大於pH 9時,則品位及回收率皆下降。此外,水相回收物中玻璃粉的品位及回收率亦隨著pH值的增加及SDS添加量的增加而上升,並在大約pH 9時,添加2.5 kg/ton SDS所達到最佳的品位為91.2%,其回收率為86%,不過,在大於pH 9時,則品位及回收率皆下降。The grade and recovery of the glass powder in the cerium oxide polishing powder and the aqueous phase recovery in the isooctane phase recovery at various pHs under the addition of 1 kg/ton and 2.5 kg/ton SDS, with the pH value The increase is increased, and at about pH 9, the best grade is 86.8% when adding 2.5 kg/ton SDS, and the recovery rate is 91.7%. However, when it is greater than pH 9, the grade and recovery rate are decreased. . In addition, the grade and recovery of the glass powder in the aqueous phase recovery also increased with the increase of pH value and the increase of SDS addition, and at the pH of about 9, the best grade was added by adding 2.5 kg/ton SDS. 91.2%, the recovery rate is 86%, however, when it is greater than pH 9, the grade and recovery rate are reduced.

另外,第四圖為上述示範性實例的分離功效,顯示pH 9下SDS添加量對異辛烷相回收物中氧化鈰拋光粉與水相回收物中玻璃粉的品位及回收率。顯而易見的是,隨著SDS添加量的增加,異辛烷相回收物中氧化鈰拋光粉與水相回收物中玻璃粉的品位及回收率皆上升,其最佳結果為添加10 kg/ton SDS,此時,異辛烷相回收物中氧化鈰拋光粉之品位達100 %,且其回收率可達94.2 %,而水相回收物中玻璃粉之品位及回收率是分別為94.6 %和100 %。氧化鈰拋光粉與玻璃粉已近乎完全分離。In addition, the fourth graph is the separation efficiency of the above exemplary examples, showing the amount of SDS added at pH 9 and the grade and recovery of the glass powder in the cerium oxide polishing powder and the aqueous phase recovery in the isooctane phase recovery. Obviously, as the amount of SDS added increases, the grade and recovery of the glass powder in the cerium oxide polishing powder and the aqueous phase recovery in the isooctane phase recovery increase, and the best result is the addition of 10 kg/ton SDS. At this time, the grade of cerium oxide polishing powder in the isooctane phase recovery is 100%, and the recovery rate is up to 94.2%, and the grade and recovery rate of the glass powder in the aqueous phase recovery are 94.6% and 100, respectively. %. The cerium oxide polishing powder is almost completely separated from the glass powder.

進一步參考第五A圖及第五B圖,如果是使用NaOL當作表面活性劑,且氧化鈰拋光粉與玻璃粉的混合重量比例為1:1。Further referring to FIGS. 5A and 5B, if NaOL is used as the surfactant, the mixing ratio of the cerium oxide polishing powder to the glass powder is 1:1.

當添加1 kg/ton及2.5 kg/ton NaOL時,在各pH下異辛烷相回收物中氧化鈰拋光粉與水相回收物中玻璃粉的品位及回收率,其中異辛烷相回收物中氧化鈰拋光粉品位及回收率是隨pH值的增加而上升,並於大約pH 7時,添加2.5 kg/ton NaOL具有最佳之品位為78.3%,其回收率為93.7%,而在大於pH 7時,品位及回收率皆接下降。再者,水相回收物中玻璃粉的品位及回收率亦隨pH值的增加而上升,其中在大約pH 7時,添加2.5 kg/ton NaOL可達到的最佳品位為91.3%,其回收率為77.4%,但是在大於pH 7時,品位及回收率皆下降。When adding 1 kg/ton and 2.5 kg/ton NaOL, the grade and recovery of the glass powder in the cerium oxide polishing powder and the aqueous phase recovery in the isooctane phase recovery at each pH, wherein the isooctane phase recovery The grade and recovery of the cerium oxide polishing powder increased with the increase of pH value. At about pH 7, the addition of 2.5 kg/ton NaOL had the best grade of 78.3%, and the recovery rate was 93.7%. At pH 7, the grade and recovery rate decreased. Furthermore, the grade and recovery of the glass powder in the aqueous phase recovery also increased with the increase of pH value, and at about pH 7, the best grade that can be achieved by adding 2.5 kg/ton NaOL was 91.3%, and the recovery rate was 91.3%. It was 77.4%, but when it was greater than pH 7, the grade and recovery rate decreased.

再如第六圖所示,在大約pH 7下,異辛烷相回收物中氧化鈰拋光粉與水相回收物中玻璃粉的品位及回收率是隨著NaOL添加量的增加而皆上升,其最佳結果是在添加7.5 kg/ton NaOL時,異辛烷相回收物中氧化鈰拋光粉之品位為94.5 %,其回收率為99 %,而水相玻璃粉之品位為99%,其回收率94.7 %。氧化鈰拋光粉與玻璃粉已近乎完全分離。As shown in the sixth figure, at about pH 7, the grade and recovery of the glass powder in the cerium oxide polishing powder and the aqueous phase recovery in the isooctane phase recovery are both increased with the addition of NaOL. The best result is that when 7.5 kg/ton NaOL is added, the grade of cerium oxide polishing powder in the isooctane phase recovery is 94.5 %, the recovery rate is 99%, and the grade of the aqueous phase glass powder is 99%. The recovery rate was 94.7%. The cerium oxide polishing powder is almost completely separated from the glass powder.

再舉出另一實例,其中捕集劑是使用DAA,而且氧化鈰拋光粉與玻璃粉是1:1混合。Another example is shown in which the collector is DAA and the cerium oxide polishing powder is 1:1 mixed with the glass powder.

如第七A圖及第七B圖所示,添加1 kg/ton及2.5 kg/ton DAA在各pH下水相回收物中氧化鈰拋光粉與異辛烷相回收物中玻璃粉的品位及回收率。在添加2.5 kg/ton DAA時,水相回收物中氧化鈰拋光粉品位及回收率隨pH值增加而上升,並於pH 9時,具有最佳之品位為72.7%,其回收率為100%,但是大於pH 9時,品位及回收率皆下降,此外,在添加2.5 kg/ton DAA時,異辛烷相回收物中玻璃粉的品位及回收率亦隨pH值的增加而上升,其中於pH 9時具有最佳之品位為98.9%,其回收率為62.7%,但是大於pH 9時,品位及回收率下降。As shown in Figures 7A and 7B, the grade and recovery of the glass powder in the cerium oxide polishing powder and the isooctane phase recovery in the aqueous phase recovery at 1 kg/ton and 2.5 kg/ton DAA were added. rate. When adding 2.5 kg/ton DAA, the grade and recovery of cerium oxide polishing powder in the aqueous retentate increased with the increase of pH value, and at pH 9, the best grade was 72.7%, and the recovery rate was 100%. However, when it is greater than pH 9, the grade and recovery rate are decreased. In addition, when adding 2.5 kg/ton DAA, the grade and recovery rate of the glass powder in the isooctane phase recovery also increase with the increase of pH value. At pH 9, the best grade was 98.9%, and the recovery was 62.7%. However, when it was greater than pH 9, the grade and recovery rate decreased.

再如第八圖所示,於pH 9下DAA添加量對水相回收物中氧化鈰拋光粉與異辛烷相回收物中玻璃粉的品位及回收率,其中隨著DAA添加量增加,水相回收物中氧化鈰拋光粉與異辛烷相回收物中玻璃粉的品位及回收率皆上升。最佳結果是在添加2.5 kg/ton DAA時,其中水相回收物中氧化鈰拋光粉之品位為72.7 %,其回收率為99.3 %,而異辛烷相玻璃粉之品位為98.9%,其回收率62.7 %。Further, as shown in the eighth figure, the DAA addition amount to the grade and recovery rate of the glass powder in the cerium oxide polishing powder and the isooctane phase recovery in the aqueous phase recovery at pH 9, wherein the water increases as the amount of DAA increases. The grade and recovery rate of the glass powder in the cerium oxide polishing powder and the isooctane phase recovery in the phase recovery increased. The best result is that when adding 2.5 kg/ton DAA, the grade of cerium oxide polishing powder in the aqueous phase recovery is 72.7 %, the recovery rate is 99.3%, and the grade of isooctane phase glass powder is 98.9%. The recovery rate was 62.7 %.

綜上所述,本發明的特點在於利用可相互分離的有機溶劑相以及水相而有效分離原始混合物中的氧化鈰拋光粉及玻璃粉,且所消耗的能源較少,尤其不會產生二次污染性廢水,因而能大幅提升整體的分離效應。In summary, the present invention is characterized in that the cerium oxide polishing powder and the glass powder in the original mixture are effectively separated by using an organic solvent phase and an aqueous phase which are separable from each other, and the energy consumed is less, especially not secondary. Polluted wastewater can greatly enhance the overall separation effect.

此外,本發明方法可對氧化鈰拋光粉與玻璃碎屑粉的混合粉體進行直接分離,並從氧化鈰玻璃拋光廢棄物中分離回收氧化鈰拋光粉,因此,除了可促進氧化鈰拋光粉的循環再利用之外,亦可做為各種稀土金屬的二次資源使用。In addition, the method of the present invention can directly separate the mixed powder of the cerium oxide polishing powder and the glass crumb powder, and separate and recover the cerium oxide polishing powder from the cerium oxide glass polishing waste, thereby, in addition to promoting the cerium oxide polishing powder. In addition to recycling, it can also be used as a secondary resource for various rare earth metals.

本發明的另一特點在於依據有機溶劑及捕集劑的特性調整最佳的酸鹼值,使得後續所添加的捕集劑能發揮最佳捕集功效,因而在有機溶劑相中或水相中能富含所需的氧化鈰拋光粉或玻璃粉。Another feature of the present invention is that the optimum pH value is adjusted according to the characteristics of the organic solvent and the trapping agent, so that the subsequently added trapping agent can exert the optimal trapping effect, and thus in the organic solvent phase or in the aqueous phase. Can be enriched with the required cerium oxide polishing powder or glass powder.

由於本發明可在一般的分離設備中實施,而不需額外設計特別的裝置,使得產業利用性相當高,非常具有市場競爭力。此外,本發明的技術並未被習用的先技術揭露,因而具有技術新穎性及進步性。Since the present invention can be implemented in a general separation apparatus without additionally designing a special device, the industrial utilization is quite high and it is very competitive in the market. Moreover, the techniques of the present invention have not been disclosed in the prior art, and thus have technical novelty and advancement.

以上所述者僅為用以解釋本發明之較佳實施例,並非企圖據以對本發明做任何形式上之限制,是以,凡有在相同之發明精神下所作有關本發明之任何修飾或變更,皆仍應包括在本發明意圖保護之範疇。The above is only a preferred embodiment for explaining the present invention, and is not intended to limit the present invention in any way, and any modifications or alterations to the present invention made in the spirit of the same invention. All should still be included in the scope of the intention of the present invention.

S10~S80‧‧‧步驟S10~S80‧‧‧Steps

G‧‧‧玻璃粉G‧‧‧Glass powder

P‧‧‧氧化鈰拋光粉P‧‧‧Oxide polishing powder

第一圖顯示依據本發明實施例氧化鈰拋光粉與玻璃粉的分離方法的示意圖。 第二圖顯示本發明的分離方法所要達成的具體功效。 第三A圖及第三B圖顯示本發明的示範性實例於不同pH值下所達成具體分離功效。 第四圖為本發明依據第三A圖及第三B圖的實例於pH9值下的分離功效。 第五A圖及第五B圖顯示本發明的另一示範性實例於不同pH值下所達成具體分離功效。 第六圖為本發明依據第五A圖及第五B圖的實例於pH7值下的分離功效。 第七A圖及第七B圖顯示本發明的另一示範性實例於不同pH值下所達成具體分離功效。 第八圖為本發明依據第七A圖及第七B圖的實例於pH9值下的分離功效。The first figure shows a schematic view of a method of separating cerium oxide polishing powder from glass frit according to an embodiment of the present invention. The second figure shows the specific efficacy to be achieved by the separation method of the present invention. Figures 3A and 3B show specific separation efficacies achieved at different pH values for an exemplary embodiment of the invention. The fourth figure is the separation efficiency of the invention according to the examples of the third A and the third B at pH 9. Figures 5A and 5B show a specific separation efficiency achieved at different pH values by another illustrative example of the invention. The sixth figure is the separation efficiency of the present invention at pH 7 according to the examples of Figs. 5A and 5B. Figures 7A and 7B show another exemplary embodiment of the invention achieving specific separation efficacies at different pH values. The eighth figure is the separation efficiency of the present invention at pH 9 according to the examples of Figs. 7A and 7B.

Claims (5)

一種氧化鈰拋光粉與玻璃粉的分離方法,包括:一前處理,加入去離子水於包含一氧化鈰拋光粉及一玻璃粉的一原始混合物中,並混合成一粉末混合漿料;一分散處理,係利用一超音波分散機以分散該粉末混合漿料中的該氧化鈰拋光粉及該玻璃粉,且該分散處理係進行二分鐘至二小時之間;一調整酸鹼值處理,係加入一酸性調整劑或一鹼性調整劑的一酸鹼值調整劑,以調整該粉末混合漿料的酸鹼值至一目標酸鹼值;一添加捕集劑處理,添加當作一界面活性劑的一捕集劑,用以對該粉末混合漿料所包含的氧化鈰拋光粉或玻璃粉產生捕集作用,而該捕集劑為一陰離子捕集劑或一陽離子捕集劑;一混合處理,利用一搖盪機所產生的搖盪力而對該粉末混合漿料進行一初階混合,且該初階混合係進行二分鐘至二小時之間,之後添加一有機溶劑,該有機溶劑是不互溶於該去離子水,並利用該搖盪機進行一進階混合而形成一粉末混合液,且該進階混合係進行二分鐘至二小時之間;一靜置處理,將該粉末混合液靜置至少二十分鐘,形成上下相互分離的一有機溶劑相溶液及一水相溶液,再分別取出該有機溶劑相溶液及該水相溶液,其中該有機溶劑相溶液及該水相溶液係分別富含該氧化鈰拋光粉或富含該玻璃粉; 一離心處理,對該有機溶劑相溶液及該水相溶液分別利用相對應的一離心機所產生的離心力,藉以分離其中的固體物及液體,並取出該固體物,該有機溶劑相溶液的固體物或該水相的固體物係包含該氧化鈰拋光粉或該玻璃粉;以及一烘乾處理,係利用一烘乾機而對該有機溶劑相溶液中所取出的該固體物或該水相中所取出的該固體物進行加熱,藉以去除殘留的液體而分別得到該氧化鈰拋光粉或該玻璃粉,其中該氧化鈰拋光粉及該玻璃粉在該原始混合物的重量比例分別為100:1至1:1之間,該目標酸鹼值為pH4至pH10之間,該捕集劑在該有機溶劑的濃度為0.5kg/ton至10.0kg/ton之間,該有機溶劑對該去離子水的重量比為100:1至1:1之間該有機溶劑包含異辛烷(isooctane)、十二烷(dodecane)或煤油(kerosine),而該捕集劑包含十二烷基硫酸鈉(Sodium Dodecyl Sulfate,SDS)、油酸鈉(Sodium Oleate,NaOL)及十二烷胺醋酸鹽(Dodecylamine Acetate,DAA)的其中之一,該捕集劑為SDS時,該目標酸鹼值為pH8.0至pH9.5之間,而該捕集劑為NaOL時,該目標酸鹼值為pH7或pH7至pH7.5之間,且該捕集劑為DAA時,該目標酸鹼值為pH8.0至pH9.5之間。 A method for separating cerium oxide polishing powder and glass powder comprises: pre-treatment, adding deionized water to an original mixture containing cerium oxide polishing powder and a glass powder, and mixing into a powder mixed slurry; Using an ultrasonic disperser to disperse the cerium oxide polishing powder and the glass powder in the powder mixed slurry, and the dispersion treatment is performed for two minutes to two hours; An acidity adjuster or a pH adjuster of an alkali adjuster to adjust the pH value of the powder mixed slurry to a target pH value; a addition of a collector treatment, added as a surfactant a trapping agent for collecting the cerium oxide polishing powder or the glass powder contained in the powder mixed slurry, and the collecting agent is an anion trapping agent or a cation trapping agent; And using a shaking force generated by a shaker to perform a preliminary mixing of the powder mixed slurry, and the preliminary mixing system is carried out for between two minutes and two hours, after which an organic solvent is added, and the organic solvent is Mutually soluble in the deionized water, and subjected to an advanced mixing by the shaker to form a powder mixture, and the advanced mixing system is carried out for between two minutes and two hours; after a static treatment, the powder mixture is allowed to stand still After being disposed for at least twenty minutes, an organic solvent phase solution and an aqueous phase solution separated from each other are formed, and the organic solvent phase solution and the aqueous phase solution are respectively taken out, wherein the organic solvent phase solution and the aqueous phase solution are respectively rich. Containing the cerium oxide polishing powder or enriching the glass powder; After centrifuging, the organic solvent phase solution and the aqueous phase solution are respectively subjected to centrifugal force generated by a corresponding centrifuge to separate the solid matter and the liquid therein, and the solid matter is taken out, and the solid solvent phase solution is solid. Or the solid phase of the aqueous phase comprises the cerium oxide polishing powder or the glass powder; and a drying treatment, the solid or the aqueous phase taken out from the solution of the organic solvent phase by using a dryer The solid material taken out is heated to remove the residual liquid to obtain the cerium oxide polishing powder or the glass powder, wherein the cerium oxide polishing powder and the glass powder have a weight ratio of 100:1 in the original mixture respectively. Between 1:1, the target acid-base value is between pH 4 and pH 10, and the concentration of the collector in the organic solvent is between 0.5 kg/ton and 10.0 kg/ton, and the organic solvent is the deionized water. The organic solvent comprises isooctane, dodecane or kerosine in a weight ratio of 100:1 to 1:1, and the collector comprises sodium lauryl sulfate (Sodium) Dodecyl Sulfate, SDS), sodium oleate (Sod One of ium Oleate, NaOL) and Dodecylamine Acetate (DAA), when the collector is SDS, the target pH value is between pH 8.0 and pH 9.5, and the capture When the concentration agent is NaOL, the target acid-base value is between pH 7 or pH 7 to pH 7.5, and when the collector is DAA, the target acid-base value is between pH 8.0 and pH 9.5. 依據申請專利範圍第1項之氧化鈰拋光粉與玻璃粉的分離方法,其中該酸性調整劑包含鹽酸及硝酸的至少其中之一,而該鹼性調整劑包含氫氧化鈉及氫氧化鉀的至少其中之一。 The method for separating cerium oxide polishing powder and glass powder according to claim 1, wherein the acid adjusting agent comprises at least one of hydrochloric acid and nitric acid, and the alkaline adjusting agent comprises at least one of sodium hydroxide and potassium hydroxide. one of them. 依據申請專利範圍第1項之氧化鈰拋光粉與玻璃粉的分離方法,其中該原始混合物具有0.2μm至~60.5μm的一粒徑範圍,且該原始混合物的平均粒徑(D50)為1.8μm至3.5μm。 a method for separating cerium oxide polishing powder and glass powder according to claim 1 of the patent application, wherein the original mixture has a particle size range of 0.2 μm to -60.5 μm, and an average particle diameter (D 50 ) of the original mixture is 1.8 Mm to 3.5 μm. 依據申請專利範圍第1項之氧化鈰拋光粉與玻璃粉的分離方法,其中該有機溶劑相溶液及該水相溶液是利用一分液漏斗而分離。 The method for separating cerium oxide polishing powder and glass powder according to claim 1 of the patent application, wherein the organic solvent phase solution and the aqueous phase solution are separated by a separatory funnel. 依據申請專利範圍第1項之氧化鈰拋光粉與玻璃粉的分離方法,其中該前處理係利用一過濾處理及/或一去油處理,以分別去除該原始混合物所包含的顆粒狀不純物質、油狀潤滑液或結劑。 a method for separating cerium oxide polishing powder and glass powder according to claim 1 of the patent application, wherein the pretreatment is performed by a filtration treatment and/or a degreasing treatment to separately remove particulate impure substances contained in the original mixture, Oily lubricating fluid or cement.
TW106132781A 2017-09-25 2017-09-25 A seperation method of cerium oxide abrasive and glass powder TWI645045B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
TW106132781A TWI645045B (en) 2017-09-25 2017-09-25 A seperation method of cerium oxide abrasive and glass powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
TW106132781A TWI645045B (en) 2017-09-25 2017-09-25 A seperation method of cerium oxide abrasive and glass powder

Publications (2)

Publication Number Publication Date
TWI645045B true TWI645045B (en) 2018-12-21
TW201915176A TW201915176A (en) 2019-04-16

Family

ID=65431695

Family Applications (1)

Application Number Title Priority Date Filing Date
TW106132781A TWI645045B (en) 2017-09-25 2017-09-25 A seperation method of cerium oxide abrasive and glass powder

Country Status (1)

Country Link
TW (1) TWI645045B (en)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI738564B (en) * 2020-11-13 2021-09-01 國立臺北科技大學 Method for separating cerium oxide abrasive from glass polishing waste

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201136709A (en) * 2010-02-15 2011-11-01 Mitsui Mining & Amp Smelting Co Ltd Recycle method of ceric abrasive

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW201136709A (en) * 2010-02-15 2011-11-01 Mitsui Mining & Amp Smelting Co Ltd Recycle method of ceric abrasive

Also Published As

Publication number Publication date
TW201915176A (en) 2019-04-16

Similar Documents

Publication Publication Date Title
JP5598631B2 (en) Recovery method of rare earth elements
Kim et al. Recovery of cerium from glass polishing slurry
JP6941229B2 (en) Rare earth concentrate treatment methods and systems
CA2948401C (en) System and process for selective rare earth extraction with sulfur recovery
CN101605717A (en) Method for producing nano lead oxide
CN109402415A (en) A kind of preparation of low grade natural rutile can chlorination rich-titanium material method
CN110241309A (en) A method for extracting white carbon black and rare earth water purifying agent from waste rare earth polishing powder
CN103215012B (en) A kind of preparation method of rare earth polishing powder regeneration
CN102275930B (en) Recycling method for silicon powder
CN107344725A (en) The preparation technology of elemental lithium in sulfuric acid straight dipping process extraction lithium ore
TWI645045B (en) A seperation method of cerium oxide abrasive and glass powder
CN102815728A (en) Method for preparing nano-sized magnesium hydroxide and nano-silica by utilization of boron mud
JP4730903B2 (en) Method for recovering raw materials for cerium-based abrasives
CN109108048B (en) Mechanochemical conversion and recovery method of sodium-containing compounds and fluorine-containing compounds in aluminum electrolysis anode carbon residue
WO2020124238A1 (en) Process for purifying a zircon sand
CN114908259B (en) Method for selectively extracting beryllium from beryllium-containing sludge based on hydrothermal ore phase regulation and control
CN114213976A (en) Method for preparing rare earth polishing powder for cover plate glass by using glass polishing waste residue particle regeneration technology
CN112676029A (en) Method for preparing water glass by using purified iron tailings
CN101979325B (en) Refining treatment method for crude zinc oxide
CN106048651A (en) Electrolytic manganese metal production method
CN1378604A (en) Method for producing metal or metal compound comprising process of treating with fluorine and adjusted raw material used therein
CN116926351A (en) Method for removing fluorine in ionic rare earth concentrate through conversion
CN115821057A (en) Resourceful treatment method for cryolite-containing secondary aluminum ash
CN1852864A (en) Process for recovering titanium dioxide from titanium-containing compositions
CN113666409A (en) A method for preparing gallium oxide by treating gallium nitride waste by acid method