TW200424123A - Method of refining phosphoric acid - Google Patents
Method of refining phosphoric acid Download PDFInfo
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- TW200424123A TW200424123A TW093107832A TW93107832A TW200424123A TW 200424123 A TW200424123 A TW 200424123A TW 093107832 A TW093107832 A TW 093107832A TW 93107832 A TW93107832 A TW 93107832A TW 200424123 A TW200424123 A TW 200424123A
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- Prior art keywords
- phosphoric acid
- solution
- exchange resin
- acid
- diluent
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 229
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 115
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000007670 refining Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000003085 diluting agent Substances 0.000 claims abstract description 40
- 239000012535 impurity Substances 0.000 claims abstract description 36
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 229910052751 metal Inorganic materials 0.000 claims abstract description 33
- 239000002184 metal Substances 0.000 claims abstract description 33
- 239000012153 distilled water Substances 0.000 claims abstract description 23
- 239000003729 cation exchange resin Substances 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 20
- 238000007865 diluting Methods 0.000 claims abstract description 12
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 83
- 239000002253 acid Substances 0.000 claims description 42
- 238000010790 dilution Methods 0.000 claims description 14
- 239000012895 dilution Substances 0.000 claims description 14
- 238000004821 distillation Methods 0.000 claims description 13
- 239000011347 resin Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 12
- 150000001768 cations Chemical class 0.000 claims description 11
- 239000003957 anion exchange resin Substances 0.000 claims description 10
- 230000004913 activation Effects 0.000 claims description 9
- 150000002500 ions Chemical class 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 239000012528 membrane Substances 0.000 claims description 5
- 238000005292 vacuum distillation Methods 0.000 claims description 4
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 claims description 3
- 239000013522 chelant Substances 0.000 claims description 3
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 claims description 3
- 235000020778 linoleic acid Nutrition 0.000 claims description 3
- 229910052778 Plutonium Inorganic materials 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 claims description 2
- OYEHPCDNVJXUIW-UHFFFAOYSA-N plutonium atom Chemical compound [Pu] OYEHPCDNVJXUIW-UHFFFAOYSA-N 0.000 claims description 2
- 239000003973 paint Substances 0.000 claims 1
- 239000003456 ion exchange resin Substances 0.000 abstract description 15
- 229920003303 ion-exchange polymer Polymers 0.000 abstract description 15
- 229910021645 metal ion Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 9
- 238000005259 measurement Methods 0.000 description 8
- 238000011084 recovery Methods 0.000 description 6
- 239000011260 aqueous acid Substances 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 4
- 239000004642 Polyimide Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 235000019197 fats Nutrition 0.000 description 4
- 125000000524 functional group Chemical group 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 150000002736 metal compounds Chemical class 0.000 description 4
- 239000011574 phosphorus Substances 0.000 description 4
- 229910052698 phosphorus Inorganic materials 0.000 description 4
- 229920001721 polyimide Polymers 0.000 description 4
- 238000005341 cation exchange Methods 0.000 description 3
- 230000006837 decompression Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- -1 Ming and Zhen Chemical class 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 150000001767 cationic compounds Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000005360 mashing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- PWEBUXCTKOWPCW-UHFFFAOYSA-N squaric acid Chemical compound OC1=C(O)C(=O)C1=O PWEBUXCTKOWPCW-UHFFFAOYSA-N 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000006277 sulfonation reaction Methods 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 229910021654 trace metal Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/02—Gases or liquids enclosed in discarded articles, e.g. aerosol cans or cooling systems of refrigerators
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C18/00—Disintegrating by knives or other cutting or tearing members which chop material into fragments
- B02C18/06—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
- B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
- B07B4/00—Separating solids from solids by subjecting their mixture to gas currents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B30—PRESSES
- B30B—PRESSES IN GENERAL
- B30B9/00—Presses specially adapted for particular purposes
- B30B9/02—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material
- B30B9/04—Presses specially adapted for particular purposes for squeezing-out liquid from liquid-containing material, e.g. juice from fruits, oil from oil-containing material using press rams
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65G—TRANSPORT OR STORAGE DEVICES, e.g. CONVEYORS FOR LOADING OR TIPPING, SHOP CONVEYOR SYSTEMS OR PNEUMATIC TUBE CONVEYORS
- B65G33/00—Screw or rotary spiral conveyors
- B65G33/08—Screw or rotary spiral conveyors for fluent solid materials
- B65G33/14—Screw or rotary spiral conveyors for fluent solid materials comprising a screw or screws enclosed in a tubular housing
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B3/00—Drying solid materials or objects by processes involving the application of heat
- F26B3/02—Drying solid materials or objects by processes involving the application of heat by convection, i.e. heat being conveyed from a heat source to the materials or objects to be dried by a gas or vapour, e.g. air
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B2101/00—Type of solid waste
- B09B2101/20—Filters, e.g. oil filters
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/58—Construction or demolition [C&D] waste
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- General Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Thermal Sciences (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
Description
200424123 五、發明說明（l) 【發明所屬之技術領域】 本發明係關於一種磷酸提煉方法，特別是關於由含金屬 雜質之工業用麟酸中分離及去除金屬雜質，而回收高純度 磷酸的一種磷酸提煉方法。 【先前技術】 藉由提煉工業用麟酸而回收高純度碟酸係一種習知技 術，其通常係選用一蒸餾法、一薄膜分離〔過濾〕法、一 離子交換樹脂處理法、一溶液萃取法等。然而，由於上述 方法之咼純度磷酸的回收率及提煉率過低而不符合經濟效 益，因而並不適合商業化用途。 、工 士具體而言，若藉由蒸餾法提煉工業用磷酸或其相似物| 寸w亥方法無法去除銘、鎮等金屬，然而可去除四I化石夕 等氟化物。 另外’若藉由美國專利第4, 277, 488號之溶液萃取法及 ，濾法提煉工業用填酸或其相似物時，由於鋁、鈣、矽、 氣、鎮等金屬雜質溶解於磷酸或含磷酸之混合酸中且無法 有效去除二因此該方法亦難以回收高純度之磷酸。’ 例士 I呂專金屬雜質，其在填酸或含構酸之混合酸中係存 ，各種化學形式，例如微粒、複合物、陽離子及陰離子 等 口此’若藉由離子交換樹脂處理法提煉金屬雜質時， 由於回收=低落，因此難以回收高純度之磷酸。 * $者’破酸基本上在酸性〔pH〕下係形成帶有陽離子之 後合2 ’其形成的複合物尺寸過大，且其帶電量會依條件 文又 因此習用離子交換樹脂處理法在碗酸的回收率上200424123 V. Description of the invention (l) [Technical field to which the invention belongs] The present invention relates to a method for refining phosphoric acid, and more particularly to a method for separating and removing metal impurities from industrial linoleic acid containing metal impurities and recovering high-purity phosphoric acid. Phosphoric acid extraction method. [Previous technology] The recovery of high-purity dishic acid by refining industrial linoleic acid is a conventional technology, which usually uses a distillation method, a membrane separation [filtration] method, an ion exchange resin treatment method, and a solution extraction method. Wait. However, because the recovery and refining rates of osmium-purified phosphoric acid are too low to be economically beneficial, they are not suitable for commercial use. In particular, if the industrial phosphoric acid or its analogs are refined by distillation, the Inch Whai method cannot remove metals such as Ming and Zhen, but it can remove fluorides such as quaternary fossils. In addition, if the solution extraction method of U.S. Patent No. 4,277,488 and the filtration method are used to refine industrial filling acid or the like, metal impurities such as aluminum, calcium, silicon, gas, and ball are dissolved in phosphoric acid or Phosphoric acid-containing mixed acids cannot be effectively removed, so this method also makes it difficult to recover high-purity phosphoric acid. '' Case I Lu special metal impurities, which exist in the filling acid or mixed acid containing acid, various chemical forms, such as particulates, composites, cations and anions, etc. 'If refined by ion exchange resin treatment In the case of metal impurities, it is difficult to recover high-purity phosphoric acid because recovery = low. * $ 者 'breaking acid is basically formed in the acidic [pH] system with cations and then 2'. The size of the complex formed is too large, and its charge will be adjusted according to the conditions and therefore the ion exchange resin treatment method is used Recovery rate
第6頁 200424123 五 發明說明 (2) 仍有 過於低落的問題。 【發明内容】 服上述習用技術之可d:煉方法’其用以克 工業用磷酸回收高純度之磷酸。义率的由含金屬雜質之 本發明提供一種磷酸提煉方法，苴 業用磷酸中有效的分離及去除金屬雜ϊ由含金屬雜質之工 石葬酸。 、”貝’以回收高純度之 、根，本發明之方法，其係在利用 進行陽離子交換處理前，i 父換樹脂對磷酸Page 6 200424123 V. Description of the invention (2) There is still a problem of too low. [Summary of the Invention] The d: refining method serving the conventional technology is used to recover high-purity phosphoric acid by using industrial phosphoric acid. The present invention provides a method for refining phosphoric acid, which effectively separates and removes metal impurities from phosphoric acid in industry, and buryes acid with metal impurities. "" Shell "to recover high-purity roots, the method of the present invention, before using the cation exchange treatment, i
.化〕鱗酸，因而該鱗酸中存：=屬處：3釋及電化學活 換樹脂所吸收。 貝可由該陽離子I 一更具體而言，本發明提供一種方法， Α 父換樹脂處理鱗酸前，將磷酸中的各「在利用陽離子 合物轉變成離子形式，以便於藉由一 形式之金屬化 及提煉。 于父換法進行分離 為達成上述目的，本發明提供一種磷酸 含電化學活化一稀釋液〔磷酸水溶液〕的=琛方法，其包 利用陽離子交換樹脂處理該稀釋液之前，^驟’该步驟在 釋石粦酸，並施加一電能至該稀釋液。 用瘵顧水稀 另外，本發明提供一種磷酸提煉方法，其勺人 驟：（a)、利用一蒸餾水稀釋含金屬雜質之下列步 之混合酸；（b)、施加一電能至該稀釋步驟^酸或含填酸 〔磷酸水溶液〕，以電化學活化該稀釋液·之稀釋液 U)、利用陽 ：:\L(XK)-5\FIVE C()NTINENTS\PF1271 .ptd 第7頁 ZUU424123 五、發明說明（3) 尚隹子父換樹脂處理 藉由減壓蒸鶴上述陽：二:活化後之稀釋液；及(d)、 收高純度之填酸。^子父換樹脂處理後之稀釋液，以回 【實施方式】 然其並非用以限制本 本發明將以下列命a , 發明之範圍。…列詳細說明 月二^第1圖所不’本發明之 苐一步驟〔稀釋步驟Ί 甘m ^ 成百无進行一 之工業用鱗酸，以勢丄=7 =水稀釋含金屬雜質.]] Scaly acid, so the squaric acid is stored in: = genus: 3 release and absorbed by the electrochemically active resin. More specifically, the present invention provides a method in which the amino acid is converted to an ionic form by using a cationic compound before the resin is treated with cations. In order to achieve the above purpose, the present invention provides a method for the electrochemical activation of a dilute solution of phosphoric acid with a phosphoric acid solution [aqueous solution of phosphoric acid], which comprises the step of treating the diluent with a cation exchange resin. 'This step releases tartaric acid, and applies an electric energy to the diluent. The water is diluted with water. In addition, the present invention provides a method for refining phosphoric acid, which comprises: (a) diluting a metal-containing impurity with distilled water; The mixed acid in the following steps; (b), applying an electric energy to the diluting step ^ acid or containing acid [aqueous solution of phosphoric acid] to electrochemically activate the diluent · Diluent U], using yang :: \ L (XK ) -5 \ FIVE C () NTINENTS \ PF1271.ptd Page 7 ZUU424123 V. Description of the invention (3) Shang Yun's father and father exchange resin treatment by decompression steaming the above-mentioned yang: 2: dilute solution after activation; and ( d), high purity Fill the acid. ^ The father and father change the diluted solution after the resin treatment to return to [Embodiment]. However, it is not intended to limit the scope of the present invention. 'The first step of the present invention [dilution step 甘 gan m ^ Hundreds of non-performing industrial scale acid, with potential 丄 = 7 = water to dilute metal impurities
I 該稀釋步驟係用二 。 率。 扠开後、呀離子父換树脂處理步驟之效 在該稀釋步驟中，其較佳調整該稀釋液， :m。㈣，釋步驟中，其較佳使用一蒸鶴:二至： 八^ '^去離子水之各種金屬雜質含量需少於l〇ppt〔兆 若由含磷酸之混合酸回收高純度之磷酸時，含磷酸之混 合酸在進行上述稀釋前，必需先在減壓下進行蒸餾，如2 可先由t磷酸之混合酸中去除磷酸以外的各種酸液。 Μ請再參照第1圖所示，本發明接著進行一第二步驟，其 藉由施加一電能至該稀釋步驟後之稀釋液〔磷酸水溶 液〕，以電化學活化該稀釋液。 、該步驟用以將該稀釋液〔磷酸水溶液〕中的各種化學形 1之金屬雜質轉變成離子形式，以便可藉由一離子交換樹 脂進行提煉。更具體而言，鋁等金屬雜質成份在該稀釋液I This dilution step is performed with two. rate. After the split, the effect of the ion-exchange resin treatment step is preferably adjusted in the dilution step,: m. ㈣ In the release step, it is preferred to use a steamed crane: two to: eight ^ '^ Deionized water must contain less than 10 ppt of various metal impurities [trillion if high purity phosphoric acid is recovered from a mixed acid containing phosphoric acid Before the above-mentioned dilution of the mixed acid containing phosphoric acid, distillation must be performed under reduced pressure. For example, various acid liquids other than phosphoric acid can be removed from the mixed acid of t phosphoric acid. Please refer to FIG. 1 again. The present invention then proceeds to a second step, which is to electrochemically activate the diluent by applying an electric energy to the dilute solution [aqueous phosphoric acid solution] after the diluting step. 5. This step is used to convert the metal impurities of various chemical forms 1 in the diluent [aqueous phosphoric acid solution] into ionic forms so that they can be refined by an ion exchange resin. More specifically, metal impurities such as aluminum are contained in the diluent.
200424123 五、發明說明（4) ~------- 物 鱗：：：液〕中係存在各種化學形式，例如微 1%離子及陰離子等，因此該電化 设口 ，種:匕學形式之金屬雜質轉變成離子形式，二 離子父換樹脂進行提煉。 9由一 二所，，為了電化學活化該稀釋液〔磷酸水 /、較侄係藉由使用一特定材料之— / ， ^ n >u %往 亚加加雷原：η 1 至10伏特、頻率50至丨，000, 〇〇〇赫兹土 · 1 〔磷酸水溶液〕。 之又抓电至该稀釋液 屬ί H:直流電取代該交流電而施加於該稀釋液，則全 =子將核在該電極之表面，因此可能減低該電極=| —請再參照第1圖所示，本發明接著進行一第三步驟，1 藉由利用陽離子交換樹脂處理上述電化學活化後之釋、 〔磷酸水溶液〕，以去除該稀釋液〔磷酸水溶液〕中之= 屬複合離子，亦即進行一陽離子交換樹脂處理步驟。此五 日年’上述使用之陽離子交換樹脂係具有一離子交換官能 基’該離子交換官能基具有適當表面密度，其符合 化學性質。200424123 V. Description of the invention (4) ~ ------- There are various chemical forms in the scales ::: liquid], such as micro 1% ions and anions, etc. Therefore, the electrochemical system has a mouth, species: The metal impurities are converted into ionic form, and the two-ion parent is changed to resin for refining. 9 From one or two institutes, in order to electrochemically activate the diluent [phosphoric acid /, compared with the neighbourhood by using a specific material— /, ^ n > u% to the Yagare source: η 1 to 10 volts The frequency is 50 to 10,000,000 Hz · 1 [aqueous phosphoric acid]. Then grab the electricity to the diluent. H: Direct current is applied to the diluent instead of the alternating current, then all = the core will be on the surface of the electrode, so it may reduce the electrode = | — Please refer to Figure 1 again In the present invention, a third step is performed. 1 By using a cation exchange resin to treat the above-mentioned electrochemically activated release, [aqueous phosphoric acid solution], to remove the diluent [aqueous phosphoric acid solution] = a complex ion, that is, A cation exchange resin treatment step is performed. In these five days, the cation exchange resin used above has an ion-exchange functional group. The ion-exchange functional group has an appropriate surface density and is in accordance with chemical properties.
上述陽離子交換樹脂處理步驟較佳係將該稀釋液〔碟酸 水溶液〕通過含陽離子交換樹脂之一濾塔或一容器。 此時，該稀釋液〔磷酸水溶液〕之流速係1 · Q SV至 5· OsV，特別是1· 5sV 至2. 5sV。 請再參照第1圖所示，本發明接著進行一第四步驟〔減 壓蒸餾步驟〕，其藉由減壓蒸餾上述陽離子交換樹脂處理The above-mentioned cation exchange resin treatment step is preferably to pass the diluent [aqueous acid solution] through a filter tower or a container containing a cation exchange resin. At this time, the flow rate of the diluted solution [aqueous solution of phosphoric acid] is from 1 · Q SV to 5 · OsV, especially from 1 · 5sV to 2.5sV. Please refer to FIG. 1 again. The present invention then proceeds to a fourth step [decompression distillation step], which is performed by distilling the above-mentioned cation exchange resin under reduced pressure.
C:\L0U0-5\1;IVU CONTINENTS\PF1271 .ptdC: \ L0U0-5 \ 1; IVU CONTINENTS \ PF1271 .ptd
200424123 五、發明說明（5) 後之稀釋液〔構酸水溶液〕，以分離及去除一蒸鶴水，進 而回收高純度之磷酸，因而完成本發明之所有步驟。上述 減壓蒸餾步驟係用以將上述提煉後之稀釋液〔磷酸水溶 液〕濃縮成高純度之磷酸，其濃度大於85%，因此該方法 較佳係在室溫至1 5 0 °C之相對低溫下使用一薄膜減壓蒸餾 法’以避免因加熱產生高黏性磷酸之聚合反應。 由該減壓蒸餾步驟所產生的蒸餾水較佳可用於上述稀釋 步驟’以達到可回收性，以供減少廢棄物及形成製程連貫 性0200424123 V. Description of the invention (5) The diluent solution [aqueous acid solution] is used to separate and remove a steamed crane water, thereby recovering high-purity phosphoric acid, thus completing all steps of the present invention. The above-mentioned reduced-pressure distillation step is used to concentrate the above-mentioned refined diluent [aqueous phosphoric acid solution] into high-purity phosphoric acid, the concentration of which is greater than 85%. Therefore, the method is preferably at a relatively low temperature from room temperature to 150 ° C. A thin film vacuum distillation method is used to avoid the polymerization reaction of high viscosity phosphoric acid generated by heating. The distilled water produced by the vacuum distillation step is preferably used in the above-mentioned dilution step to achieve recyclability for reducing waste and forming process coherence.
請筝照第2圖所示，其揭示本發明另一磷酸提煉方法> 該方法可在經由一高分子多孔性薄膜過濾磷酸後，再利% 一蒸餾水稀釋磷酸。另一方面，利用一蒸餾水稀釋磷酸而 製得之稀釋液〔磷酸水溶液〕亦可在經由一高分子多孔性 薄膜的過濾後，再進行電化學活化。 在上述方法中，磷酸較佳係在該稀釋步驟之前，先經由 一高分子多孔性薄膜進行過遽。 該過濾步驟係用以減少後續離子交換樹脂處理步驟之離 子交換能力的負載。Please refer to Figure 2, which discloses another phosphoric acid refining method of the present invention. The method can filter the phosphoric acid through a polymer porous membrane and then dilute the phosphoric acid with distilled water. On the other hand, the dilute solution [aqueous phosphoric acid solution] prepared by diluting phosphoric acid with distilled water can also be electrochemically activated after filtering through a polymer porous membrane. In the above method, it is preferable that the phosphoric acid is subjected to a sulfonation through a polymer porous film before the dilution step. This filtration step is used to reduce the load on the ion exchange capacity of the subsequent ion exchange resin treatment step.
該高分子多孔性薄膜可由各種高分子所製成，例如聚亞 醯胺〔polyimide〕、聚醯胺〔p〇lyamide〕、鐵氟龍 〔Teflon〕及其相似物，該薄膜之孔徑較佳係1〇龍至〇· 5 β m 〇 再者，在該過濾、製程中，該 2000psig〔石旁/平方英叶〕， 壓力較佳係1 〇 〇 p s i g至 該溫度較佳係室溫至80 °C。The polymer porous film can be made of various polymers, such as polyimide, polyamide, Teflon, and the like. The pore diameter of the film is preferably 〇long to 0.5 β m 〇 In addition, in the filtering and manufacturing process, the 2000 psig [stone side / square inch leaf], the pressure is preferably 100 psig to the temperature, preferably room temperature to 80 ° C.
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請參照第3圖所示’其揭示本發明再—磷酸提煉方法。 =方法利用-蒸餾水稀釋磷酸而製得之稀釋液〔磷酸水溶 液〕可在進行電化學活化前，先選擇利用陽離子交換樹 月旨：陰離子交換樹脂、陽離子及陰離子交換樹脂之混合物 或益合物樹脂加以處理。另—方s，該稀釋液〔磷酸水溶 液〕亦可先進行電化學活化，再選擇利用陽離子交換樹 脂、陰離子交換樹脂、陽離子及陰離子交換樹脂之混合物 或螯合物樹脂加以處理。Please refer to FIG. 3 ', which discloses the re-phosphoric acid refining method of the present invention. = Method The diluent [aqueous phosphoric acid solution] prepared by diluting phosphoric acid with distilled water can be used to select the cation exchange tree before electrochemical activation: anion exchange resin, a mixture of cation and anion exchange resin or a beneficial resin To deal with. On the other hand, the diluted solution [aqueous solution of phosphoric acid] can also be electrochemically activated first, and then treated with a cation exchange resin, anion exchange resin, a mixture of cation and anion exchange resin, or a chelate resin.
上述步驟使用之各種離子交換樹脂較佳具有一官能某， 該官能基具有適當表面密度，其適合用以去除極微量^金 屬化合物。 I、 該稀釋液〔磷酸水溶液〕通過離子交換樹脂之流速較4 係 l.OsV 至 5.0sV，特別是 1.5sV 至 2.5sV。 在利用一蒸餾水稀釋該磷酸前，該磷酸可經由該高分子 多孔性薄膜進行過遽，另一方面，亦可在利用一蒸=二稀 釋該蒸顧過濾液〔高濃度之磷酸〕的步驟後，再使該稀釋 液〔構酸水溶液〕經由該高分子多孔性薄膜進行過^。The various ion exchange resins used in the above steps preferably have a functional group, and the functional group has an appropriate surface density, which is suitable for removing a very small amount of metal compounds. I. The flow rate of the diluted solution [aqueous phosphoric acid solution] through the ion exchange resin is l.OsV to 5.0sV, especially 1.5sV to 2.5sV. Before diluting the phosphoric acid with a distilled water, the phosphoric acid may be subjected to mashing through the polymer porous film. On the other hand, after the step of diluting the distilled solution [high concentration phosphoric acid] with one distillation = two Then, the diluted solution [aqueous acid solution] is passed through the polymer porous film.
如上所述，本發明利用一蒸餾水稀釋含金屬雜質磷酸， 以製備一稀釋液〔磷酸水溶液〕。接著，在該稀釋液利用 陽離子父換樹脂處理前’其係先施加一電能於該稀釋液而 進行電化學活化，如此將該稀釋液中的金屬化合物之化學 形式轉變成離子形式，以供藉由一離子交換法進行分離: 因此可有效的分離及去除該金屬雜質。 結果’本發明可去除填酸中超過9 9 %之金屬雜質，因此As described above, the present invention uses a distilled water to dilute phosphoric acid containing metal impurities to prepare a dilute solution [aqueous phosphoric acid solution]. Then, before the diluent is treated with a cationic parent resin, it first applies an electric energy to the diluent for electrochemical activation, so that the chemical form of the metal compound in the diluent is converted into an ionic form for borrowing. Separation by an ion exchange method: Therefore, the metal impurities can be effectively separated and removed. Result 'The present invention can remove more than 99% of the metal impurities in the filling acid, so
200424123 五、發明說明（7) )m 可回收高純度之磷酸，並控制金屬雜質含量至小於1 0PPI 〔百萬分之一〕。 上述回收之高純度攝酸可用於一紹钱刻液之組成物，其 應用於單晶石夕晶圓製程、半導體製程或TFT-LCD〔薄膜電 晶體液晶顯示器〕製程等領域。 第一實施例： 含各種金屬雜質〔總含量7〇PPm〕之工業用磷酸係在室 温及5 0 0碎/平方英吋的壓力下利用一聚亞醯胺多孔性薄 膜〔孔徑0 · 4 // m〕進行過濾。 接著’過濾後之磷酸係利用一蒸餾水進行稀釋，因而學 得一稀釋液含有濃度1 7%之磷酸。 接著’該稀釋液〔磷酸水溶液〕通過含陽離子及阶離子 ii”物的—濾塔’“進行離子交換樹脂處；。該 稀釋，〔蛳酸水溶液〕的流速係2· OsV。 、、存接^番上述離子交換樹脂處理後之稀釋液〔磷酸水溶 液係置入—水槽中，該水槽設有一電極，a # # ^ 1伏特、頻率〗nnn姑# 具係使用電壓 稀釋液〔碟酸水=;〕之。一交流電’因而可電化學活化該 過=離化r稀釋液〔填酸水溶液〕係通 理，因而去除塔’以進行陽離子交換樹脂處 〔磷，水溶液〕的流速係2.0sV。 巧稀釋液200424123 V. Description of the invention (7)) m can recover high purity phosphoric acid, and control the content of metal impurities to less than 10PPI [parts per million]. The above-recovered high-purity photoacid can be used for the composition of a etched liquid, which is used in the fields of monocrystalline wafer process, semiconductor process, or TFT-LCD [thin film liquid crystal display] process. First Example: An industrial phosphoric acid system containing various metal impurities [total content of 70 PPm] utilizes a polyimide porous film at a room temperature and a pressure of 500 pieces per square inch [pore diameter 0 · 4 / / m] for filtering. Subsequently, the filtered phosphoric acid was diluted with a distilled water, and it was learned that a diluted solution contained phosphoric acid at a concentration of 17%. Next, "the diluted solution [aqueous solution of phosphoric acid] passes through a filter column containing cations and secondary ions ii", and then proceeds to an ion exchange resin; In this dilution, the flow rate of the aqueous solution of osmic acid was 2. OsV. 2. Store the diluted solution after the above ion exchange resin treatment [the phosphoric acid aqueous solution is placed in a water tank, which is provided with an electrode, a # # ^ 1 volt, frequency〗 nnn 姑 # with the use of voltage diluent [ Dish sour water =;] of it. An alternating current 'thus electrochemically activates the ionization [diluted solution [acid-filled aqueous solution]] system, and thus removes the column' to carry out the [phosphorus, aqueous solution] flow rate at the cation exchange resin at 2.0 sV. Clever diluent
液接ί置i述，離子交換樹脂處理後之稀釋液〔碟酸水溶 係置入一減壓蒸鶴器中，並在之減壓下進HThe liquid connection is described, the diluted solution after the ion exchange resin treatment [disc acid water solution is placed in a decompression steamer, and it is fed under reduced pressure.
：：\ΚΧίΟ-5\Ηΐνΐΐ C0NT1NENTS\PF1271 .ρ1(ι 第12頁 200424123 五、發明說明（8) I留，以分離成南純 餾液〔蒸餾水〕係 成回收高純度之磷 上述回收〔提煉 結果係列於下列表 第二實施例： 含各種金屬雜質 一蒸德水進行稀釋 有濃度1 7%之磷酸£ 接著，該稀釋液 設有一電極，其係 流電，因而可電化 接著，上述電化 過含陽離子交換樹 理，因而去除該稀 〔磷酸水溶液〕的 接著，上述陽離 液〕係置入一減壓 餾，以分離成高純 餾液〔蒸餾水〕係 成回收高純度之磷 上述回收〔提煉 結果係列於下列表 第三實施例： 〔>5粦酸水 使用電壓 學活化該 學活化後 脂的一遽 釋液中的 流速係2. 子交換樹 蒸餾器中 度之磷酸 可供應及 酸。 〕之磷酸 度之磷酸及一蒸餾液〔蒸餾水〕，該蒸 可供應及回收用於該稀釋步驟，因此完 酸。 〕之磷酸所含的金屬雜質總含量的測量 〔總含量70ppm〕之工業用磷酸係利用 ，因而製得一稀釋液〔填酸水溶液〕含 溶液〕係置入一水槽，該水_ 1伏特、頻率1 0 0 0赫茲之一交 稀釋液〔碌酸水溶液〕。 之稀釋液〔磷酸水溶液〕係通 i合’以進行陽離子父換樹脂處 微量金屬雜質離子。該稀釋液 OsV ° 脂處理後之稀釋液〔磷酸水溶 ，並在1 0 0 °c之減壓下進行蒸 及一蒸餾液〔蒸餾水〕，該蒸 回收用於該稀釋步驟，因此完 所含的金屬雜質總含量的測量：: \ ΚΧίΟ-5 \ Ηΐνΐΐ C0NT1NENTS \ PF1271 .ρ1 (ι Page 12 200424123 V. Description of the invention (8) I remain, separated into South pure distillate [distilled water] system to recover high purity phosphorus as described above [refined The series of results are shown in the second example below. Distilled water containing various metal impurities is diluted with 17% phosphoric acid. Next, the diluted solution is provided with an electrode, which is galvanic, so it can be electrified. Contains cation exchange tree structure, so the dilute [aqueous phosphoric acid solution] is removed. Then, the above-mentioned positive ion solution is put into a vacuum distillation to separate into a high-purity distillate [distilled water] to recover high-purity phosphorus. The series of results are shown in the third example of the following table: [> The flow rate of 5 粦 acid water using a voltaic method to activate the sterilized fat release solution is 2. The moderate phosphoric acid supply and acid in the sub-exchange tree still .] Phosphoric acid with a degree of phosphoric acid and a distillate [distilled water], the steam can be supplied and recovered for use in the dilution step, so the acid is complete.] Measurement of the total content of metal impurities contained in phosphoric acid A total of 70 ppm] of industrial phosphoric acid is used, so a diluent [acid-filled aqueous solution] containing solution] is prepared and placed in a water tank. The water _ 1 volt and a frequency of 100 Hz are cross-diluted. Aqueous acid solution]. The diluent solution [aqueous solution of phosphoric acid] is used to exchange trace metal impurity ions at the cation parent exchange resin. This dilution solution is OsV ° The diluent solution after the fat treatment [water soluble in phosphoric acid and at 100 ° C Distillation and a distillate [distilled water] are performed under reduced pressure, and the distillation is used for the dilution step, so the measurement of the total content of metal impurities is completed
C: \ LOCK) - 5 \ l·' IVI: CONTINENTS \ PF1 2 71. p t d 第13頁 200424123 五、發明說明（9) 含各種金屬雜夤〔總含量7 〇 ppm〕之工業用磷酸係利用 一蒸餾水進行稀釋，因而製得一稀釋液〔磷酸水溶液〕含 有濃度1 7 %之叾粦酸。 接著，上述製得之瘵餾過濾液〔高濃度磷酸〕係在室溫 及50 0ySig〔碌/平方英时〕的壓力下利用一聚亞醯胺多 孔性薄膜〔孔徑0 · 4 // m〕進行過淚。 接著’上述過濾後之稀釋液〔鱗酸水溶液〕通過含陽離 子及陰離子交換樹脂混合物的一濾塔，以進行離子交換樹 脂處，。該稀釋液〔磷酸水溶液〕的流速係2. 〇sV。 接著，上述離子交換樹脂處理後之稀釋液〔磷酸水溶 液、〕係置入一水槽中，該水槽設有一電極，其係使用電 H特/頻+率1 000赫兹之—交流電，因而可電化學活化該 稀釋液〔碟酸水溶液〕。 、ft雙二錐ΐ述電化學活化後之稀釋液〔磷酸水溶液〕係通 it，m ^二柃的一濾塔，以進行陽離子交換樹脂處 矛、该稀釋液中的微量金屬 〔填，水溶液〕的流速係2 0^里。至屬雜貝離子。邊稀釋液 液〕係置入ί:3 =換樹脂處理後之稀釋液〔磷酸水溶 德，以分離成高；：；；：，ΐ在1〇°。°之減壓下進行蒸 餾液〔蒸餾水〕係〇 +次及一蒸餾液〔蒸餾水〕，該蒸 成回收高純声> 及回收用於该稀釋步驟，因此完 & 石拜酸。 上述回收〔提 結果係列於下列主 W s欠所含的金屬雜質總含量的測量 夕j 表一 〇C: \ LOCK)-5 \ l · 'IVI: CONTINENTS \ PF1 2 71. ptd page 13 200424123 V. Description of the invention (9) Industrial phosphoric acid system containing various metal impurities (total content 70 ppm) Distilled water was used to dilute, so that a dilute solution [aqueous phosphoric acid solution] containing osmic acid at a concentration of 17% was prepared. Next, the above-mentioned retort filtrate [high-concentration phosphoric acid] was prepared by using a polyimide porous film [pore diameter 0 · 4 // m] at room temperature and a pressure of 50 μsig [hours per square inch]. Tears. Next, the above-mentioned filtered diluent [aqueous scale acid solution] is passed through a filter tower containing a mixture of cations and anion exchange resins to perform an ion exchange resin. 〇sV。 The flow rate of the diluted solution [aqueous phosphoric acid] is 2.0 sV. Next, the diluted solution [aqueous solution of phosphoric acid,] after the above ion exchange resin treatment is placed in a water tank, which is provided with an electrode, which uses an electric current of H terahertz / frequency + rate of 1,000 Hz-alternating current, so it can be electrochemically This diluent [aqueous acid solution] is activated. Ft, double dipyramid, the dilute solution [aqueous phosphoric acid solution] after electrochemical activation is a filter column through it, m ^ dipyridine, to carry out the cation exchange resin treatment, trace metals in the diluent [filled, aqueous solution The flow velocity is 20 ^ miles. To the miscellaneous shell ions. The side diluent solution] is placed in ί: 3 = the resin-diluted diluent solution [phosphoric acid is dissolved in water to separate into high;:;, ΐ at 10 °. Distillation [distilled water] is performed at a reduced pressure of 0 ° and one distillate [distilled water] is used. This distillation recovers high-purity sound and recovers it for the dilution step. The above recovery (the results are shown in the following series of measurements of the total content of metal impurities contained in the main ions). Table 1 〇
第14頁 200424123 五、發明說明（10) 第四實施例： 業用磷酸係在室 含各種金屬雜質〔總含量7〇ppm〕之工業用 溫及5 0 0ysig〔磅/平方英吋〕的壓力下利用_聚亞醉 多孔性薄膜〔孔徑〇 · 4 v ^〕進行過濾。 1 一接著：上述過濾後之蒸餾過濾液〔高濃度磷酸〕係利用 瘵餾水進仃稀釋，因而製得一稀釋液含有濃度丨之粆 酸。 夕牛 接著，上述製得之稀釋液〔磷酸水溶液〕係置入一 中，該水槽設有一電極，其係使用電壓i伏特、 曰 % 2茲，一交流電，因而可電化學活化該稀釋液〔磷酸水 ，耆，上述電化學活化後之稀釋液〔 脂的一渡塔，以進行陽離子交^ r β ΐ稀釋液中的微量金屬雜質離子。該稀釋液 〔磷？水溶液〕的流速係2.0sV。 釋液 说ί Ϊ i ^離子交換樹脂處理後之稀釋液〔石粦酸水溶液〕 二、=匕陽離子及陰離子交換樹脂混合物的一濾塔，以進 2灯0^子交換樹脂處理。該稀釋液〔磷酸水溶液〕的流速係 接著、，、離ί交換樹脂處理後之稀釋液〔磷酸水溶液〕係 ，广、^壓瘵餾器中，並在10 〇 °c之減壓下進行蒸餾，以 刀，成问純度之磷酸及一蒸餾液〔蒸餾水〕，該蒸餾液 〔，餾水〕係可供應及回收用於該稀釋步驟，因此完成回 收高純度之碟酸。 _ C:\LOCiO-5\FIVH CONTINENTS\PFI27I. pid 第15頁 200424123 五、發明說明（π) 上述回收〔提煉〕之填酸所含的金屬雜質總含量的測量 結果係列於下列表一。 第一比較實施例： 將上述第一實施例之工業用磷酸在相同第一實施例之製 程及條件下進行提煉，但不進行電化學活化該稀釋液〔磷 酸水溶液〕之步驟，以回收〔提煉〕高純度之磷酸。 上述回收〔提煉〕之磷酸所含的金屬雜質總含量的測量 結果係列於下列表一。 第二比較實施例： 將上述第二實施例之工業用磷酸在相同第二實施例之製^ 程及條件下進行提煉，但不進行電化學活化該稀釋液〔磷 酸水溶液〕之步驟，以回收〔提煉〕高純度之磷酸。 上述回收〔提煉〕之磷酸所含的金屬雜質總含量的測量 結果係列於下列表一。 第三比較實施例： 具10 0 Oppm金屬雜質〔例如鋁〕之工業用磷酸係在室溫 及5 0 Ops ig〔磅/平方英吋〕的壓力下利用一聚亞醯胺多 孔性薄膜〔孔徑0. 4 // m〕進行過濾，因而回收〔提煉〕磷 酸。 上述回收〔提煉〕之磷酸所含的金屬雜質總含量的測量 結果係列於下列表一。Page 14 200424123 V. Description of the invention (10) The fourth embodiment: The industrial phosphoric acid type contains various metal impurities [total content of 70 ppm] in the industrial temperature of 50 0 sig [pounds per square inch] pressure It was filtered using a polyarsenic porous film [pore size 0.4 V ^]. 1 Next: The above-mentioned filtered distillate filtrate [high concentration phosphoric acid] is diluted with distillate water, thereby preparing a dilute solution containing dilute acid. Xi Niu next, the above-prepared diluent [aqueous phosphoric acid solution] was put into one, and the water tank was provided with an electrode, which used a voltage i volt,% 2 volts, and an alternating current, so that the diluent could be electrochemically activated [ Phosphoric acid water, plutonium, the above-mentioned diluted solution after electrochemical activation [fat of a fat tower, to carry out cationic cross-linking β r ΐ dilute metal impurity ions in the diluted solution. The diluent [phosphorus? The flow rate of the aqueous solution] was 2.0 sV. Release solution Said ί Ϊ ^ dilute solution after treatment with ion exchange resin [aqueous solution of osmic acid] Second, a filter tower containing a mixture of cations and anion exchange resins, and treated with 2 lamps. The flow rate of the dilute solution [aqueous phosphoric acid solution] is followed by, and the dilute solution [aqueous phosphoric acid solution] after the exchange resin treatment is performed, and the distillation is performed under a reduced pressure of 100 ° C. in a wide-range pressure distillation machine. With a knife, the purity of phosphoric acid and a distillate [distilled water] can be supplied and recovered for the diluting step, so the recovery of high-purity dishic acid is completed. _ C: \ LOCiO-5 \ FIVH CONTINENTS \ PFI27I. Pid page 15 200424123 V. Description of the invention (π) The measurement of the total content of metal impurities contained in the above-mentioned recovered [refined] filling acid is shown in Table 1 below. First comparative embodiment: The industrial phosphoric acid of the first embodiment is refined under the same process and conditions of the first embodiment, but the step of electrochemically activating the diluted solution [phosphoric acid aqueous solution] is not performed to recover the [refining 〔High purity phosphoric acid. The measurement results of the total content of metallic impurities contained in the recovered [refined] phosphoric acid are listed in Table 1 below. Second comparative embodiment: The industrial phosphoric acid of the second embodiment is refined under the same manufacturing process and conditions of the second embodiment, but the step of electrochemically activating the diluted solution [aqueous phosphoric acid solution] is not performed to recover [Refined] High-purity phosphoric acid. The measurement results of the total content of metallic impurities contained in the recovered [refined] phosphoric acid are listed in Table 1 below. Third Comparative Example: An industrial phosphoric acid system with 100 Oppm metal impurities (such as aluminum) uses a polyimide porous film [pore diameter 0. 4 // m] is filtered, so [refined] phosphoric acid is recovered. The measurement results of the total content of metallic impurities contained in the recovered [refined] phosphoric acid are listed in Table 1 below.
C:\LOGO-5\FIVE C()NTINENTS\PF1271. ptd 第16頁 200424123 五、發明說明（12) 表一、各截刻液中金屬雜質含量之測量結果〔ppm〕 瓣J/ppm 在使用的 含鱗酸刻液中 在回收的 含鱗SHi刻液中 第一實施例 70 0Ό1 第二實施例 70 0Ό2 第三實施例 70 0.02 第四實施例 70 0Ό3 第一比較實施例 70 0.25 第二比較實施例 70 0.34 第三實施例 70 0.50 本發明確實可由含各種金屬化合物〔例如鋁〕之磷酸中 有效的去除及分離金屬化合物，而以一極高效率順利回收 高純度之磷酸。 雖然本發明已利用較佳實施例詳細揭示，然其並非用以 限定本發明，任何熟習此技藝者，在不脫離本發明之精神 和範圍内，當可作各種更動與修改，因此本發明之保護範 圍當視後附之申請專利範圍所界定者為準。C: \ LOGO-5 \ FIVE C () NTINENTS \ PF1271. Ptd page 16 200424123 V. Description of the invention (12) Table I. Measurement results of metal impurity content in each truncated solution [ppm] flap J / ppm in use Of the scale-containing acid solution in the recovered scale-containing SHi solution First example 70 0Ό1 Second example 70 0Ό2 Third example 70 0.02 Fourth example 70 0Ό3 First comparative example 70 0.25 Second comparison Example 70 0.34 Third Example 70 0.50 The present invention can indeed effectively remove and separate metal compounds from phosphoric acid containing various metal compounds such as aluminum, and smoothly recover high purity phosphoric acid with a very high efficiency. Although the present invention has been disclosed in detail using preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. The scope of protection shall be determined by the scope of the attached patent application.
C:\LOCK)-5\FIVH C0NTINENTS\PF1271.ptd 第17頁 200424123C: \ LOCK) -5 \ FIVH C0NTINENTS \ PF1271.ptd Page 17 200424123
C: \ LOGO - 5 \ FIVI: CONTINENTS \ ΡΡΊ 2 71. p l d 第18頁C: \ LOGO-5 \ FIVI: CONTINENTS \ ΡΡΊ 2 71. p l d p.18
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| CH701939B1 (en) * | 2007-09-06 | 2011-04-15 | Sulzer Chemtech Ag | Method and apparatus for the purification of aqueous phosphoric acid. |
| KR101600184B1 (en) * | 2014-07-18 | 2016-03-07 | 오씨아이 주식회사 | Purification of phosphoric acid |
| KR102633772B1 (en) * | 2018-04-12 | 2024-02-05 | 오씨아이 주식회사 | Method for preparing high purity phosphoric acid |
| CN115631992A (en) * | 2022-11-04 | 2023-01-20 | 北京化学试剂研究所有限责任公司 | Boron-aluminum diffusion source and preparation method thereof |
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