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Method and apparatus for obtaining purified phosphoric acid from phosphoric acid aqueous solution containing plural metal ions

A technology of phosphoric acid aqueous solution and metal ions, which is applied in the direction of phosphoric acid, phosphorus oxyacids, non-metallic elements, etc., can solve the problems of unrecorded coprecipitation, etc., and achieve the effect of stabilizing the etching process and reducing the supply amount

Inactive Publication Date: 2008-08-13
NIPPON REFINE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0011] However, Non-Patent Document 2 only describes the general co-precipitation phenomenon, and does not describe the co-precipitation of metal ions in concentrated phosphoric acid as in the present invention at all.

Method used

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  • Method and apparatus for obtaining purified phosphoric acid from phosphoric acid aqueous solution containing plural metal ions
  • Method and apparatus for obtaining purified phosphoric acid from phosphoric acid aqueous solution containing plural metal ions
  • Method and apparatus for obtaining purified phosphoric acid from phosphoric acid aqueous solution containing plural metal ions

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Experimental program
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Embodiment 1

[0089] The recycling system shown in FIG. 3 was used to treat the mixed acid aqueous solution waste liquid in the Al etching process. In addition, the unit of the component is "kg", and "N.D." means below the lower limit of detection.

[0090] The composition of the mixed acid aqueous solution waste liquid (about 100 kg) discharged from the etching step is as follows. Metal ions other than Al and Mo are negligible because they are in extremely small amounts.

[0091] Table 1

[0092] phosphoric acid

[0093] In addition, the composition of the distillate (about 27.8 kg) from the evaporator is as follows.

[0094] Table 2

[0095] phosphoric acid

[0096] In addition, the composition of concentrated phosphoric acid (about 72.2 kg) passed through the evaporator is as follows.

[0097] table 3

[0098] phosphoric acid

[0099] Next, dissolve 7.4 kg of sodium dihydrogen phosphate in 10 kg of water, add to the crystallization and co-precipitation ...

Embodiment 2

[0124] The treatment of the mixed acid aqueous solution waste liquid of the Al etching process similar to Example 1 was performed.

[0125] The composition of the mixed acid aqueous solution waste liquid (about 100kg) discharged from the etching process, the composition of the distillate (about 27.8kg) from the evaporator, and the composition of the concentrated phosphoric acid (about 72.2kg) passing through the evaporator are the same as in Example 1. .

[0126] Next, the same operation as in Example 1 was carried out except that the inorganic salt was changed to 4.43 kg of sodium sulfate and dissolved in 18 kg of water for use. The composition of the treatment liquid (about 354.6 kg) at this stage is as follows.

[0127] In addition, the relationship between the amount of Na and the amount of inorganic substances is the same as in Example 1.

[0128] Table 10

[0129] phosphoric acid

water

Inorganic matter

IPA

Al

Mo

(Na)

65

...

Embodiment 3

[0141] Using the recirculation system shown in FIG. 3 , it was carried out in the same manner as in Example 1, and the treatment of the mixed acid aqueous solution waste liquid in the Al etching step was performed. Fig. 4 is a diagram showing the material budget for each basic block.

[0142] In this embodiment, in order to keep the metal ion concentration (the total amount of Al, Mo, Na) of the mixed acid aqueous solution tank below 500ppm by weight, and make the treatment capacity of the mixed acid aqueous solution waste liquid be 100kg / hour, recirculate The mixed acid aqueous solution is 90kg / hour, and the metal ion concentration of the recycled mixed acid aqueous solution is suppressed below 30ppm on a weight basis. In the case of supplementing 10kg / hour of mixed acid aqueous solution (replenishment), the upper limit of the amount of etched metal is as follows: 0.0473kg / hour.

[0143] 100kg / hour×0.0005-100kg / hour×0.9×0.00003=0.0473kg / hour

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Abstract

Method and apparatus for obtaining purified phosphoric acid from phosphoric acid aqueous solution containing plural metal ions A method for obtaining purified phosphoric acid from a phosphoric acid aqueous solution containing a plurality of metal ions includes: [1] crystallizing and coprecipitating that separate out an inorganic salt crystal from a phosphoric acid aqueous solution containing a plurality of metal ions and coprecipitate metal ions including: (a) mixing a phosphoric acid aqueous solution containing a plurality of metal ions with an inorganic salt aqueous solution; (b) separatingout an inorganic salt crystal and coprecipitating simultaneously the metal ions by further mixing an organic poor solvent which is soluble in phosphoric acid and does not dissolve an inorganic salt with the above resultant mixture; and (c) solid-liquid separating by filtering the inorganic salt crystal containing the metal ions; and [2] evaporating that obtains purified phosphoric acid by evaporating an organic poor solvent and water in a filtrate obtained by the filtration, wherein the amount of metal ions dissolved in the phosphoric acid / organic poor solvent mixture in the separating is less than the amount of metal ions in the phosphoric acid solution used in the mixing.

Description

technical field [0001] The mixed aqueous solution of nitric acid-acetic acid-phosphoric acid (hereinafter referred to as mixed acid aqueous solution) used in the metal etching process, etc., has a concentration above the use limit in etching (usually, about 500 to 1000 ppm by weight) as the content. The waste liquid of a kind of metal ion is discharged, and the present invention relates to remove metal ion from such mixed acid aqueous solution (hereinafter referred to as mixed acid aqueous solution waste liquid) etc. containing multiple metal ions, obtains the method and the device of refining phosphoric acid. In particular, it relates to a method and an apparatus suitable for treating an aqueous phosphoric acid solution, which is a residual phosphoric acid aqueous solution obtained by performing primary treatment by a melt crystallization method, a solvent extraction method, etc. (now, these phosphoric acid aqueous solutions are discarded as they are) treatment) is an aqueous...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/234
CPCC01B25/18C23F1/46
Inventor 前田正吾竹山友洁小田昭昌水谷荣一川濑泰人
Owner NIPPON REFINE
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