CN1940100B - Neutralization method of rh hydrochloric acid solution - Google Patents

Neutralization method of rh hydrochloric acid solution Download PDF

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CN1940100B
CN1940100B CN2006101057820A CN200610105782A CN1940100B CN 1940100 B CN1940100 B CN 1940100B CN 2006101057820 A CN2006101057820 A CN 2006101057820A CN 200610105782 A CN200610105782 A CN 200610105782A CN 1940100 B CN1940100 B CN 1940100B
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hydrochloric acid
neutralization
acid solution
corrective
acid soln
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CN1940100A (en
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薄井正治郎
伊东义夫
冈岛伸明
关根和广
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JX Nippon Mining and Metals Corp
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Nippon Mining and Metals Co Ltd
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Abstract

Provided is a method for obtaining a neutralized product having adequate filtration properties, when adding an alkali to an aqueous hydrochloric acid solution of Rh containing a heavy metal or an aqueous hydrochloric acid solution of Rh to neutralize and precipitate Rh and other components contained in the aqueous solution. The method for neutralizing a hydrochloric acid solution of Rh to obtain a neutralized product capable of being filtered at a high rate includes adding the alkali to the aqueous hydrochloric acid solution of Rh or the aqueous hydrochloric acid solution of Rh containing theheavy metal so that the neutralized solution produces a yellow neutralized precipitate, when neutralizing and precipitating Rh and other components contained in the aqueous solution.

Description

The neutralization method of Rh hydrochloric acid soln
Technical field
The present invention relates to contain the solution of Rh, for example, contain the intermediate residue the operation that reclaims precious metal from cupric electrolysis mucus is handled and the Rh hydrochloric acid soln of the heavy metal that obtains and the Rh hydrochloric acid soln that contains impurity hardly that obtains from this liquid is purified, neutralization precipitation reclaims the method for Rh.
Background technology
As mentioned above, with in the alkali and the hydrochloric acid soln of Rh and the technology that Rh reclaims as the corrective precipitation for example is disclosed in the spy opens 2004-332041 " recovery method of highly purified platinum group metal " (patent documentation 1) and the spy opens among the 2005-97695 " process for mutual separation of platinum group metal element " (patent documentation 2).
But the filterableness of the neutralization precipitation thing of Rh is poor sometimes, and the technology of the filterableness of unexposed this corrective of control.
They find the inventor: the filterableness of Rh corrective, according in and the color of the Rh corrective that obtains of the hydrochloric acid soln of Rh different and difference significantly.
[patent documentation 1] spy opens 2004-332041 " recovery method of highly purified platinum group metal "
[patent documentation 2] spy opens 2005-97695 " process for mutual separation of platinum group metal element "
Summary of the invention
The invention provides in a kind of aqueous hydrochloric acid and the aqueous hydrochloric acid of Rh at the Rh that contains heavy metal, add alkali, make when Rh and other composition neutralization precipitation, obtain the method for the good corrective of filterableness.
The inventor etc. have made following invention in order to address the above problem.
That is, the invention provides a kind of neutralization method of Rh hydrochloric acid soln as described below,
(1) in containing the Rh aqueous hydrochloric acid of Rh, add alkali, make when the Rh neutralization precipitation,
Interpolation speed by the aqueous sodium hydroxide solution that will use as neutralizing agent, Rh hydrochloric acid soln with respect to 1L, under situation about converting with 100 quality %NaOH, be set at more than the 13g/min, obtaining the fast xanchromatic of filtration velocity is the neutralization precipitation thing of principal constituent with Rh.
(2) in neutralization method (1), except Rh, also contain other heavy metal in the described Rh aqueous hydrochloric acid, by adding above-mentioned alkali, make described Rh and other composition neutralization precipitation.The neutralization method of Rh hydrochloric acid soln of the present invention,
(1) in alkali and when the Rh hydrochloric acid soln, by the addition means of appropriate employing alkali, the corrective of Rh becomes yellow, thereby can accelerate the filtration velocity of corrective.
(2) by extremely easy method, can access the good throw out of filterableness.
Description of drawings
Fig. 1 represent the Rh hydrochloric acid soln in and a mode of schema.
Fig. 2 represents that relative NaOH (be scaled 100 quality % and expression) adds the filtration velocity of liquid after the neutralization of speed.
Embodiment
Below, explain the present invention.
Discoveries such as the inventor: to the aqueous hydrochloric acid of Rh and the aqueous hydrochloric acid interpolation alkali that contains the Rh of heavy metal, in and Rh and other composition and the Rh corrective that obtains, difference according to the color of corrective has bigger difference, in the color according to the neutralization precipitation thing on filtration velocity, when commercial size enforcement filtration, sometimes filterableness worsens, so that filters the difficulty that becomes, on the other hand, by obtaining the xanchromatic corrective, can accelerate filtration velocity.
And then, carried out with keen determination research at neutralization method, the consequently clear and definite following fact:, can control color, the filtration velocity of corrective by the interpolation speed of the alkali that adds as neutralizing agent.
By accelerating the speed of the interpolation alkali in the neutralization operation, the corrective of Rh becomes yellow, under this situation, can accelerate filtration velocity.
The reason of the colour-change of Rh corrective is indefinite, but is well known that as the oxyhydroxide of 3 valencys, has Rh 2O 3XH 2O (x=1~5), the variation of inferring this hydration number has caused the variation of the color and the character of corrective.
By flowchart text the present invention as shown in Figure 1.The analysis of each metal ingredient of embodiment and comparative example is all undertaken by ICP emission spectroanalysis device.
[embodiment one]
To use as the preceding liquid of neutralization as the Rh hydrochloric acid soln 409ml as shown in table 1 of raw material.
[table 1]
Figure DEST_PATH_G200610105782001D00031
At fluid temperature is under the situation of room temperature, with the 24 quality %NaOH aqueous solution with the neutralization of every 1L before liquid phase to the interpolation speed of 163ml/min, be that the interpolation speed of 163ml/L/min is added to until pH and reached 7.If be scaled 100 quality %NaOH, the interpolation speed of Ci Shi NaOH then is reset at the ratio with the 24 quality %NaOH aqueous solution under 1.22 the condition, becomes 48g/L/min.Then, be heated to 90 ℃, add the 24 quality %NaOH aqueous solution once more,, place then and cool off a night pH regulator to 7.Then, through by 5C filter paper vacuum filtration neutralization precipitation thing, obtained xanchromatic Rh neutralization precipitation thing.The filtration velocity of this moment is 1087L/h/m 2At this, filtration velocity is represented with following formula.
Filtration velocity (L/h/m 2)=amount of filtrate (L) ÷ filtration time (h) ÷ filtration area (m 2)
Again, the analytical value of liquid is as shown in table 2 after Ci Shi the neutralization.The Rh rate of recovery to corrective is more than 99.9%.
[table 2]
[embodiment two]
To use as the preceding liquid of neutralization as the Rh hydrochloric acid soln 409ml as shown in table 1 of raw material.Be under 80 ℃ the situation at fluid temperature, add the 24 quality %NaOH aqueous solution to pH with the interpolation speed of 46ml/L/min (is 13g/L/min) under situation about converting with 100 quality %NaOH and reach 7, be heated to 90 ℃ then, add the 24 quality %NaOH aqueous solution once more, pH is adjusted to 7, place then and cool off a night.Through by 5C filter paper vacuum filtration neutralization precipitation thing, obtained xanchromatic Rh neutralization precipitation thing.Again, Ci Shi filtration velocity is 768L/h/m 2
Again, the analytical value of liquid is as shown in table 3 after Ci Shi the neutralization.
[table 3]
Figure S061A5782020060807D000041
The Rh rate of recovery to corrective is more than 99.9%.
[comparative example 1]
To use as the preceding liquid of neutralization as the Rh hydrochloric acid soln 12.9L as shown in table 1 of raw material.At fluid temperature is under the situation of room temperature, add the 24 quality %NaOH aqueous solution to pH with the interpolation speed of 5ml/L/min (is 1.5g/L/min) under situation about converting with 100 quality %NaOH and reach 7, be heated to 90 ℃ then, add the 24 quality %NaOH aqueous solution once more, with pH regulator to 7, place then and cool off a night.Through by 5C filter paper vacuum filtration neutralization precipitation thing, obtained orange soft Rh neutralization precipitation thing.The filtration velocity of this moment is 19L/h/m 2, very little.
Again, the analytical value of liquid is as shown in table 4 after Ci Shi the neutralization.
[table 4]
Figure S061A5782020060807D000042
The Rh rate of recovery to corrective is more than 99.9%.
[comparative example 2]
To use as the preceding liquid of neutralization as the Rh hydrochloric acid soln 409ml as shown in table 1 of raw material.Be under 90 ℃ the situation, to add the 24 quality %NaOH aqueous solution to pH with the interpolation speed of 3ml/L/min (is 0.9g/L/min) under situation about converting with 100 quality %NaOH and reach 7 at fluid temperature, place one night of cooling then.Through by 5C filter paper vacuum filtration neutralization precipitation thing, obtained orange Rh neutralization precipitation thing.The filtration velocity of this moment is 183L/h/m 2
Again, the analytical value of liquid is as shown in table 5 after Ci Shi the neutralization.
[table 5]
Figure S061A5782020060807D000051
The Rh rate of recovery to corrective is more than 99.9%.
The result of embodiment one, two and comparative example one, two is put in order as table 6 and shown in Figure 2.
[table 6]
100%NaOH adds speed (g/L/min) Fluid temperature when adding NaOH (℃) The color of corrective Filtration velocity (L/h/m 2)
Embodiment one 48 Room temperature Yellow 1087
Embodiment two 13 80 Yellow 768
Comparative example one 1.5 Room temperature Orange 19
Comparative example two 0.9 90 Orange 183
With this, can know: in the neutralization operation of Rh hydrochloric acid soln, no matter the fluid temperature of solution how before the neutralization, by making the interpolation speed of the NaOH aqueous solution, be in more than the 13g/L/min that converts with 100 quality %NaOH, can both obtain filtration velocity is 768L/h/m 2Above filtration velocity.
[embodiment three]
To use as the preceding liquid of neutralization as the Rh hydrochloric acid soln 16.1L that contains heavy metal as shown in table 7 of raw material.At fluid temperature is under the situation of room temperature, add the 24 quality %NaOH aqueous solution to pH with the interpolation speed of 125ml/L/min (is 37g/L/min) under situation about converting with 100 quality %NaOH and reach 7, be heated to then until 90 ℃, add the 24 quality %NaOH aqueous solution once more, with pH regulator to 7, place then and cool off a night.
[table 7]
Figure S061A5782020060807D000061
Through passing through 5C filter paper vacuum filtration neutralization precipitation thing, obtained the neutralization precipitation thing that is principal constituent with virellous xanchromatic Rh.The filtration velocity of this moment is 490L/h/m 2, with the embodiment one of the Rh hydrochloric acid soln that do not contain impurity of having neutralized and embodiment two similarly, obtain the fast corrective of filtration velocity.
Again, the analytical value of liquid is as shown in table 7 after Ci Shi the neutralization.The Rh rate of recovery to corrective is more than 99.9%.
By above embodiment one, two, three as can be known, adding alkali to the aqueous hydrochloric acid of the Rh that contains heavy metal and the aqueous hydrochloric acid of Rh, make when Rh and other composition neutralization precipitation, can access the fast corrective of filtration velocity, in addition, Rh is not also almost to the liquid filtrate loss of neutralization back.

Claims (2)

1. the neutralization method of a Rh hydrochloric acid soln is characterized in that,
In containing the Rh aqueous hydrochloric acid of Rh, add alkali, make when the described Rh neutralization precipitation,
Interpolation speed by the aqueous sodium hydroxide solution that will use as neutralizing agent, Rh hydrochloric acid soln with respect to 1L, under situation about converting with 100 quality %NaOH, be set at more than the 13g/min, obtaining the fast xanchromatic of filtration velocity is the neutralization precipitation thing of principal constituent with Rh.
2. the neutralization method of Rh hydrochloric acid soln as claimed in claim 1 is characterized in that,
Except Rh, also contain other heavy metal in the described Rh aqueous hydrochloric acid,, make described Rh and other composition neutralization precipitation by adding above-mentioned alkali.
CN2006101057820A 2005-09-29 2006-07-26 Neutralization method of rh hydrochloric acid solution Expired - Fee Related CN1940100B (en)

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JP5569415B2 (en) * 2011-01-28 2014-08-13 住友金属鉱山株式会社 Process for separating copper and rhodium from a raw material containing copper and rhodium

Citations (1)

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Publication number Priority date Publication date Assignee Title
CN1031567A (en) * 1987-08-13 1989-03-08 中国有色金属工业总公司昆明贵金属研究所 The dissolving and the purification of thick rhodium and high rhodium-containing alloyed scrap

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1031567A (en) * 1987-08-13 1989-03-08 中国有色金属工业总公司昆明贵金属研究所 The dissolving and the purification of thick rhodium and high rhodium-containing alloyed scrap

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