CN106430114A - Production method of sodium thiosulfate pentahydrate - Google Patents
Production method of sodium thiosulfate pentahydrate Download PDFInfo
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- CN106430114A CN106430114A CN201610915875.3A CN201610915875A CN106430114A CN 106430114 A CN106430114 A CN 106430114A CN 201610915875 A CN201610915875 A CN 201610915875A CN 106430114 A CN106430114 A CN 106430114A
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- liquor
- water
- filter cake
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- filtrate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/64—Thiosulfates; Dithionites; Polythionates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/04—Oxides; Hydroxides
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- Engineering & Computer Science (AREA)
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Abstract
The invention relates to a production method of sodium thiosulfate pentahydrate. The method is characterized by comprising the following steps: (1) adding water into an elemental sulfur-containing slag material, stirring and washing, filtering and separating to obtain a filter cake A and filtrate A; (2) adding sodium sulfite and water into the filter cake A, wherein the adding amount of the sodium sulfite is 1.1-1.2 times of a theoretical value, and the adding amount of the water is 15-20 times of the mass of the sulfur-containing slag material; carrying out agitation leaching on an obtained mixture under the condition of heating; after that, filtering and washing to obtain a precious metal-containing filter cake B and filtrate B; evaporating the filtrate B, carrying out cooling crystallization and spillover, filtering and separating, and drying to obtain the sodium thiosulfate pentahydrate. After the production method is adopted, valuable elements are effectively recycled, and two products, i.e., the sodium thiosulfate pentahydrate and sodium sulfate are obtained.
Description
Technical field
The present invention relates to technical field of wet metallurgy, and in particular to a kind of production method of five water sodium thiosulfate.
Background technology
The method of five water sodium thiosulfate of traditional mode of production is but this side using high-purity sulfur and sodium sulfite raw material
Method is but existed and requires material purity height, the unfavorable factor such as production cost is big.
With the expanding day of coloured hydrometallurgy commercial production scale, after chlorine phase analysis, the earth of positive pole, hot filtering residue hydrometallurgy
Substantial amounts of slag charge containing elemental sulfur is produced, containing substantial amounts of elemental sulfur and a small amount of noble metal in slag charge containing elemental sulfur, content is respectively
In S 50-90%, Ag 22-109g/t, Au 37.3-59.25g/t, Pd 18.93-27.75g/t, Pt 23.70-35.74g/t.
However, the utilization of sulfur is single in sulfur compound and slag charge containing elemental sulfur, it is only used for sulphuric acid is prepared, thus results in sulphuric acid
Excess production capacity increases, the low unfavorable situation of added value.Therefore in order to change this unfavorable situation, those skilled in the art
How fully to the utilization of sulfur in slag charge containing elemental sulfur, the aspects such as product diversification, added value more Gao Hua are enable to do
Positive effort is gone out.Such as：Can it be one of them that slag charge containing elemental sulfur be utilized to produce five water sodium thiosulfate.But, profit
Five water sodium thiosulfate products are produced with the slag charge containing elemental sulfur after chlorine phase analysis, hot filtering residue, earth of positive pole hydrometallurgy, be but faced with
Contained by slag charge, element is many, and complicated, produces a product difficulty difficult problem up to standard.
Content of the invention
The purpose of the present invention is aiming at the deficiency of above-mentioned prior art presence, provides a kind of using the production of slag charge containing elemental sulfur five
The method of water sodium thiosulfate.
The present invention is achieved by the following technical solutions：
A kind of production method of five water sodium thiosulfate, it is characterised in that methods described step includes：
（1）To containing elemental sulfur slag charge in add water, agitated washing, be separated by filtration after obtain filter cake A and filtrate A；
（2）Sodium sulfite and water is added in filter cake A, and wherein, the addition of sodium sulfite is 1.1-1.2 times of theoretical value, water
Addition be 15-20 times containing elemental sulfur slag charge, mixed material is carried out heated and stirred leaching；Then carry out filter with
Washing, obtains filter cake B and the liquor B containing noble metal；Liquor B is evaporated, crystallisation by cooling, overflow, be separated by filtration, dry,
Obtain five water sodium thiosulfate.
According to above-mentioned method, it is characterised in that step（2）By mixed material at a temperature of 80 DEG C, heated and stirred
Leach 3.5h.
According to above-mentioned method, it is characterised in that step（2）Baking temperature is 35 DEG C.
According to above-mentioned method, it is characterised in that carry out mixed material after heated and stirred leaching, molten to obtained
Liquid carries out pH value detection, when pH value ＞ 8 and solution are white translucent shape, adds the slag charge containing elemental sulfur, by solution pH value
Adjust to 7-8；When pH value ＜ 7 and solution be pale yellow transparent shape, add sodium sulfite, solution pH value is adjusted to 7-8.
According to above-mentioned method, it is characterised in that by step（1）Filtrate A as washings, slag charge containing elemental sulfur is entered
Row repetitive cycling is washed, is separated by filtration, and obtains liquor C, adds NaOH solution to adjust the pH value of liquor C, Ran Houjin in liquor C
Row precipitation, overflow, be separated by filtration, obtain filter cake C and filtrate D；Exposure to Sunlight, overflow, filtration will be carried out after filtrate D and overflowing liquid mixing
Separate, obtain sodium sulfate crystal.
According to above-mentioned method, it is characterised in that liquor C concentration is 10g/l.
According to above-mentioned method, it is characterised in that in liquor C add concentration by mass percentage 10% NaOH molten
Liquid, the pH value for adjusting liquor C is 9-10.
According to above-mentioned method, it is characterised in that filter cake C is Ni, Cu, Co hydroxide.
The Advantageous Effects of the present invention, the invention provides a kind of production method of five water sodium thiosulfate, by stirring
Mix washing, solid-liquid separation first the solable matter in slag charge containing elemental sulfur to be separated, then by sodium sulfite is added, reclaim slag
Elemental sulfur in material, obtains five water sodium thiosulfate of major product and the filter cake containing noble metal, by adjusting solution PH, obtains sulfur
Sour sodium and the filter cake containing Ni, Cu, Co hydroxide.The method of the present invention, makes full use of the slag charge containing elemental sulfur, effectively reclaims
Valuable element, and obtained five water sodium thiosulfate and two kinds of products of sodium sulfate.Using production efficiency of the present invention height, slag charge is made
Refuse reclamation, economizes on resources, reduces production cost and protect environment.
Description of the drawings
Fig. 1 is the process chart of the present invention.
Specific embodiment
As shown in figure 1, a kind of production method of five water sodium thiosulfate, step includes：
（1）To containing elemental sulfur slag charge in add water, agitated washing, be separated by filtration after obtain filter cake A and filtrate A；
（2）To step（1）Sodium sulfite and water is added in the filter cake A for obtaining, and wherein, the addition of sodium sulfite is theoretical value
1.1-1.2 times, the addition of water is 15-20 times containing elemental sulfur slag charge, and by mixed material at a temperature of 80 DEG C, heating is stirred
Leaching 3.5h is mixed, pH value detection is carried out to the solution for obtaining, when pH value ＞ 8 and solution are white translucent shape, add containing list
The slag charge of matter sulfur, solution pH value is adjusted to 7-8；When pH value ＜ 7 and solution be pale yellow transparent shape, add sodium sulfite, will
Solution pH value is adjusted to 7-8；Then carry out filtering, wash filter cake B and the liquor B for obtaining containing noble metal；Liquor B is steamed
Send out, crystallisation by cooling, overflow, be separated by filtration, dry, baking temperature be 35 DEG C, obtain five water sodium thiosulfate；
By step（1）Filtrate A carry out repetitive cycling washing to slag charge containing elemental sulfur, be separated by filtration as washings, filtered
Liquid C, preferably liquor C concentration are 10g/l, add the NaOH solution that concentration by mass percentage is 10% to adjust filter in liquor C
The pH value of liquid C, then carries out precipitating, overflow, is separated by filtration, obtain filter cake C and filtrate D, filter cake C for Ni, Cu, Co hydroxide
Thing；Exposure to Sunlight, overflow will be carried out after filtrate D and overflowing liquid mixing, be separated by filtration, obtain sodium sulfate crystal.
Embodiment 1
Slag charge containing elemental sulfur：S 66.25%、Na2SO4 12%, Ag 50.9g/t, Au 46.38g/t, Pd 23.46g/t, Pt
31.82g/t.Slag charge containing elemental sulfur being placed in the beaker with agitating device, water being added toward in beaker, the addition of water is
10 times containing elemental sulfur slag charge of butt, after stirring 30min, is separated by filtration, and obtains filter cake A and filtrate of the main component for elemental sulfur
A, continues to add sodium sulfite and water toward in the beaker equipped with filter cake A, and sodium sulfite addition is 1.15 times of theoretical amount,
The addition of water is 17 times of the weight of slag charge containing elemental sulfur, and mixed liquor beaker is placed in water-bath, sodium sulfite and elemental sulfur
At a temperature of 80 DEG C, heated and stirred leaches 3.5h, and detection solution PH is 7-8 and solution is colorless and transparent, through solid-liquid separation,
Obtain filter cake B and the liquor B containing noble metal, liquor B through evaporation and concentration, cooling and crystallization, overflow, filter and separate, obtain
Crystalline solid is dry at a temperature of 35 DEG C to be prepared into five water sodium thiosulfate of product；Elemental sulfur slag charge will be contained pass through with water agitator treating
Filtering isolated filtrate A as washings, the repetitive cycling of slag charge containing elemental sulfur to be washed, is separated by filtration, concentration is obtained for 10g/l
Liquor C, while liquor C is stirred, add the NaOH solution that concentration is 10% to adjust solution PH is 9.5, produces precipitation after standing,
Through overflow, it is separated by filtration, through evaporating brine and overflowing after the filter cake C for obtaining is Ni, Cu, Co hydroxide, filtrate D and overflowing liquid mixes
Stream, filtration and isolated sodium sulfate crystal side-product.The response rate of elemental sulfur is 83%.
Embodiment 2
The composition of slag charge containing elemental sulfur is with example 1.Slag charge containing elemental sulfur is placed in the beaker with agitating device, is added toward in beaker
Enter water, the addition of water contains 10 times of elemental sulfur slag charge for butt, after stirring 30min, be separated by filtration, it is single to obtain main component
The filter cake A of matter sulfur slag charge and filtrate A, continues to add sodium sulfite and water, sodium sulfite addition toward in the beaker equipped with filter cake A
For 1.2 times of theoretical amount, the addition of water is 20 times of the weight of slag charge containing elemental sulfur, and mixed liquor beaker is placed in water-bath
Interior, at a temperature of 80 DEG C, heated and stirred leaches 3.5h, detection solution PH ＞ 8 and solution is white translucent shape, to continuously add and contain
Elemental sulfur slag charge, solution PH is adjusted to 7-8 and solution is colorless and transparent, through solid-liquid separation, obtain the filter containing noble metal
Cake B and liquor B, liquor B through evaporation and concentration, cooling and crystallization, overflow, filter with separate, the crystalline solid that obtains is in 35 DEG C of temperature
Lower drying is prepared into five water sodium thiosulfate of product；Elemental sulfur slag charge will be contained it will be separated by filtration with water agitator treating and will obtain filtrate A
Repetitive cycling washing being carried out to slag charge containing elemental sulfur, is separated by filtration as washings, obtains liquor C of the concentration for 10g/l, stirring
It is 9 to add the NaOH solution that concentration is 10% to adjust solution PH while mixing liquor C, produces precipitation, through overflow, filtration after standing
Separate, the filter cake C for obtaining be after Ni, Cu, Co hydroxide and filtrate D, filtrate D and overflowing liquid mixing through evaporating brine with overflow,
Filter and isolated sodium sulfate crystal side-product.The response rate of elemental sulfur is 84%.
Embodiment 3
The composition of slag charge containing elemental sulfur is with example 1.Slag charge containing elemental sulfur is placed in the beaker with agitating device, is added toward in beaker
Enter water, the addition of water contains 10 times of elemental sulfur slag charge for butt, after stirring 30min, be separated by filtration, it is single to obtain main component
The filter cake A of matter sulfur and filtrate A, continues to add sodium sulfite and water toward in the beaker equipped with filter cake A, and sodium sulfite addition is reason
By 1.1 times of amount of calculation, the addition of water is 15 times of the weight of slag charge containing elemental sulfur, and mixed liquor beaker is placed in water-bath,
At a temperature of 80 DEG C, heated and stirred leaches 3.5h, detection solution PH ＜ 7 and solution is pale yellow transparent shape, to continuously add sulfurous
Solution PH is adjusted to sour sodium 7-8 and solution is colorless and transparent, through solid-liquid separation, obtains filter cake B and the filter containing noble metal
Liquid B, liquor B through evaporation and concentration, cooling and crystallization, overflow, filter with separate, the crystalline solid that obtains dries at a temperature of 35 DEG C and makes
Standby become five water sodium thiosulfate of product；Elemental sulfur slag charge will be contained be separated by filtration with water agitator treating filtrate A will be obtained as washing
Water to the repetitive cycling of slag charge containing elemental sulfur wash, be separated by filtration, obtain concentration for 10g/l liquor C, stirring liquor C, same
When add concentration be 10% NaOH solution adjust solution PH be 10.0, after standing produce precipitation, through overflow, be separated by filtration, obtain
Filter cake C be after Ni, Cu, Co hydroxide and filtrate D, filtrate D and overflowing liquid mixing through evaporating brine with overflow, filter and separate
Obtain sodium sulfate crystal side-product.The response rate of elemental sulfur is 85%.
Claims (8)
1. a kind of production method of five water sodium thiosulfate, it is characterised in that methods described step includes：
（1）To containing elemental sulfur slag charge in add water, agitated washing, be separated by filtration after obtain filter cake A and filtrate A；
（2）Sodium sulfite and water is added in filter cake A, and wherein, the addition of sodium sulfite is 1.1-1.2 times of theoretical value, water
Addition be 15-20 times containing elemental sulfur slag charge, mixed material is carried out heated and stirred leaching；Then carry out filter with
Washing, obtains filter cake B and the liquor B containing noble metal；Liquor B is evaporated, crystallisation by cooling, overflow, be separated by filtration, dry,
Obtain five water sodium thiosulfate.
2. the method according to claims 1, it is characterised in that step（2）By mixed material at a temperature of 80 DEG C,
Heated and stirred leaches 3.5h.
3. the method according to claims 1, it is characterised in that step（2）Baking temperature is 35 DEG C.
4. the method according to claims 1, it is characterised in that carry out mixed material after heated and stirred leaching,
PH value detection is carried out to the solution for obtaining, when pH value ＞ 8 and solution are white translucent shape, the slag charge containing elemental sulfur is added,
Solution pH value is adjusted to 7-8；When pH value ＜ 7 and solution be pale yellow transparent shape, add sodium sulfite, solution pH value is adjusted
To 7-8.
5. the method according to claims 1, it is characterised in that by step（1）Filtrate A as washings to contain simple substance
Sulfur slag charge carries out repetitive cycling washing, is separated by filtration, and obtains liquor C, adds NaOH solution to adjust the PH of liquor C in liquor C
Value, then carries out precipitating, overflow, is separated by filtration, obtain filter cake C and filtrate D；Will filtrate D and overflowing liquid mixing after carry out Exposure to Sunlight,
Overflow, it is separated by filtration, obtains sodium sulfate crystal.
6. the method according to claims 5, it is characterised in that liquor C concentration be.
7. the method according to claims 5, it is characterised in that add concentration by mass percentage 10% in liquor C
NaOH solution, adjust liquor C pH value be 9-10.
8. the method according to claims 5, it is characterised in that filter cake C be.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610915875.3A CN106430114A (en) | 2016-10-21 | 2016-10-21 | Production method of sodium thiosulfate pentahydrate |
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| CN201610915875.3A CN106430114A (en) | 2016-10-21 | 2016-10-21 | Production method of sodium thiosulfate pentahydrate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205580A (en) * | 2013-04-19 | 2013-07-17 | 金川集团股份有限公司 | Desulfurization method in noble metal enriching process |
| CN103498052A (en) * | 2013-10-11 | 2014-01-08 | 金川集团股份有限公司 | Method for efficiently enriching rare precious metals from complex low-grade heat filter residues |
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- 2016-10-21 CN CN201610915875.3A patent/CN106430114A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103205580A (en) * | 2013-04-19 | 2013-07-17 | 金川集团股份有限公司 | Desulfurization method in noble metal enriching process |
| CN103498052A (en) * | 2013-10-11 | 2014-01-08 | 金川集团股份有限公司 | Method for efficiently enriching rare precious metals from complex low-grade heat filter residues |
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Application publication date: 20170222 |