CN114835157B - Method for reducing chloride ion content in sodium stannate production process - Google Patents
Method for reducing chloride ion content in sodium stannate production process Download PDFInfo
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- CN114835157B CN114835157B CN202210418918.2A CN202210418918A CN114835157B CN 114835157 B CN114835157 B CN 114835157B CN 202210418918 A CN202210418918 A CN 202210418918A CN 114835157 B CN114835157 B CN 114835157B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for reducing chloride ion content in the production process of sodium stannate, which comprises the following steps: and (3) placing the sodium stannate initial product in an ultrasonic cleaning tank, sequentially adding glycerol, water, absolute ethyl alcohol, water and absolute ethyl alcohol into the initial product for ultrasonic cleaning, standing, filtering and drying to obtain the high-purity sodium stannate product. The adoption of the invention can reduce the chloride ion content in the sodium stannate product to less than 0.01 percent. The method is simple and effective, clean and pollution-free, and the washing liquid can be regenerated and recycled, so that a new method is provided for reducing chloride ions in the sodium stannate production process, and the method is suitable for large-scale production.
Description
Technical Field
The invention relates to the field of deep processing of nonferrous metal products, in particular to a method for reducing chloride ion content in a sodium stannate production process.
Background
Sodium stannate (Na) 2 SnO 3 ) As a chemical product for tin deep processing, it has been widely used in alkaline electroplating. At present, in industrial production, sodium stannate is generally prepared by carrying out high-temperature reaction on tin-containing materials and sodium hydroxide under the condition of an oxidant, however, due to the diversification of impurity ions of the tin-containing materials, especially chloride ions are difficult to separate in sodium stannate products, and the quality of the sodium stannate products is seriously influenced. With the improvement of product quality in the electroplating industry, the chlorine content in sodium stannate is required to be below 0.01%. In industrial production, the chlorine content of the sodium stannate product is generally more than 0.1%, so that a method for reducing the chlorine content of the sodium stannate product is sought, the method is used for preparing a high-purity sodium stannate product, the product quality is improved, the market customer requirements are met, and the method has a certain practical significance.
A great deal of research work is done for removing chloride ions at home and abroad, and chemical precipitation methods, ion exchange technology, electrochemical technology and other methods, such as a porous filler method, a water washing method, a roasting method and the like, are mainly carried out.
Chinese patent CN104961153A discloses a process for preparing superfine sodium nano stannate, which comprises filtering stannous hydroxide and using 2m 3 The washing was performed 15 times with hot water at 55 ℃. The method has the advantages of high energy consumption, long time of repeated cleaning and no chloride ion content of the finally obtained sodium stannate product being lower than 0.01 percent.
Chinese patent CN111547824a discloses a method for removing chloride ions from reclaimed water and a method for preparing an electrode, wherein activated carbon fiber is used as a negative electrode, titanium dioxide and polyaniline carbon are loaded as positive electrodes, and under the action of an electric field, chloride ions in raw water move to the positive electrodes and are adsorbed on the positive electrodes, and as the chloride ions are enriched to the positive electrodes, the chloride ions in the raw water are gradually removed. Although the activated carbon fiber has a certain electro-adsorption effect, the resistance and mass transfer resistance of the activated carbon fiber are relatively large, the electrode adsorption performance is to be improved and enhanced, and the activated carbon fiber is not suitable for large-scale application.
Disclosure of Invention
The invention aims to provide a method for reducing the chloride ion content in the sodium stannate production process, which can reduce the concentration of chloride ions without introducing impurities, ensures the purity of products and accelerates the drying time, and adopts the organic solvent which can be recycled and reused, thereby having the characteristics of simple process, safety, effectiveness and environmental protection.
In order to achieve the above purpose, the technical scheme of the invention is as follows: a method for reducing chloride ion content in sodium stannate production process comprises the following specific steps:
(1) Placing a sodium stannate initial product with chloride ion content less than 1% into an ultrasonic cleaning tank;
(2) Primary washing: preparing glycerol and water into a washing liquid according to the mass ratio of 10% -40%, pouring the washing liquid into a washing tank, ultrasonically washing for 2-5min, and then discharging the washing liquid;
(3) And (3) secondary washing: preparing washing liquid from absolute ethyl alcohol and water according to the mass ratio of 40% -60%, pouring the washing liquid into a cleaning tank, ultrasonically cleaning for 2-5min, and then discharging the washing liquid;
(4) Three times of washing: directly pouring absolute ethyl alcohol into a cleaning tank, ultrasonically cleaning for 5-10min, and standing;
(5) Filtering and drying: and rapidly filtering the sodium stannate after three times of washing, transferring into a vacuum drying oven, keeping the temperature at 60-90 ℃ for 1-2h, and drying to obtain the product.
The sodium stannate initial product in the step (1) has the crystal volume accounting for 80-90% of the total volume and the chloride ion content less than 1%.
And (3) washing in the step (2), wherein the proportion of the glycerol in the washing liquid is 10% -40%, the ultrasonic power is 100-240W, and the ultrasonic time is 2-5min.
And (3) the secondary washing, wherein the proportion of ethanol in the washing liquid is 40% -60%, the ultrasonic power is 100-240W, and the ultrasonic time is 2-5min.
And (3) washing for three times, wherein the ultrasonic power is 240-300W, and the ultrasonic time is 5-10min.
And (3) in the drying process in the step (5), the vacuum degree is-0.1 MPa, the temperature is 60-90 ℃, the preferable temperature is 75-85 ℃, the time is 1-2h, and finally the sodium stannate product with the chloride ion content less than 0.01% is obtained. The content of chloride ions in the sodium stannate product is detected to be 0.007% -0.009%.
The percentages stated in the invention are mass percentages except for the other description, and the sum of the percentages of the components is 100%.
Compared with the prior art, the invention has the beneficial effects that:
1. by utilizing the characteristic that sodium chloride is dissolved in water and glycerol and sodium stannate is insoluble in an organic solvent, the air is isolated, the ultrasonic treatment is adopted to accelerate uniform mixing, the glycerol and the water are utilized to remove chloride ions, and finally, absolute ethanol is used to wash out residual glycerol. The method not only ensures the purity of the product, but also accelerates the drying time, and finally obtains the sodium stannate product with the chloride ion content less than 0.01 percent.
2. The adopted organic solvent can be recycled, the process is simple, and the method is safe and effective.
Detailed Description
The technical scheme of the present invention is described in further detail below with reference to examples.
Example 1
This example is an example of the method for reducing chloride ion content in sodium stannate production process according to the present invention, comprising the steps of:
(1) Placing 50kg of sodium stannate initial product with 90% of crystal volume and 0.38% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Primary washing: pouring 1kg of glycerol and 9kg of water into a cleaning tank, performing ultrasonic treatment with 240W power for 2min, and immediately discharging the cleaning solution;
(3) And (3) secondary washing: pouring 5kg of absolute ethyl alcohol and 5kg of water into a cleaning tank, performing ultrasonic treatment for 2min at 240W power, and immediately discharging the cleaning solution;
(4) Three times of washing: pouring 20kg of absolute ethyl alcohol directly into a cleaning tank, performing ultrasonic treatment for 8min at 300W power to ensure that the ethyl alcohol is fully contacted with the crystal, and standing for 5min;
(5) And (3) rapidly filtering the sodium stannate crystal after three times of washing, and drying at the constant temperature of 80 ℃ for 1h under the vacuum degree of-0.1 MPa.
The weighed sodium stannate product has the mass of 43.8kg, the chloride ion content is detected to be 0.008%, and the washing liquid is recycled. The content of the detected chloride ions is 0.009%, 0.008%, 0.007%,
Example 2
This example is another example of the method for reducing chloride ion content in sodium stannate production process according to the present invention, comprising the steps of:
(1) Placing 50kg of sodium stannate initial product with 90% of crystal volume and 0.46% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Primary washing: pouring 2kg of glycerol and 8kg of water into a cleaning tank, performing ultrasonic treatment with 200W power for 2min, and immediately discharging the cleaning solution;
(3) And (3) secondary washing: pouring 4kg of absolute ethyl alcohol and 6kg of water into a cleaning tank, performing ultrasonic treatment for 3min at 200W power, and immediately discharging the cleaning solution;
(4) Three times of washing: directly pouring 20kg of absolute ethyl alcohol into a cleaning tank, performing ultrasonic treatment with power of 250W for 10min to ensure that the absolute ethyl alcohol is fully contacted with the crystal, and standing for 5min;
(5) And (3) rapidly filtering the sodium stannate crystal after three times of washing, and drying at the constant temperature of 80 ℃ for 1h under the vacuum degree of-0.1 MPa.
The weighed sodium stannate product has the mass of 40.2kg, the chloride ion content is detected to be 0.009%, and the washing liquid is recycled.
Example 3
This embodiment is another example of the method for reducing chloride ion content in sodium stannate production process according to the present invention, comprising the steps of:
(1) Placing 50kg of sodium stannate initial product with 90% of crystal volume and 0.43% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Primary washing: pouring 3kg of glycerol and 7kg of water into a cleaning tank, performing ultrasonic treatment at 150W for 5min, and immediately discharging the cleaning solution;
(3) And (3) secondary washing: pouring 6kg of absolute ethyl alcohol and 4kg of water into a cleaning tank, performing ultrasonic treatment for 3min at 150W power, and immediately discharging the cleaning solution;
(4) Three times of washing: pouring 20kg of absolute ethyl alcohol directly into a cleaning tank, performing ultrasonic treatment for 5min at 300W power to ensure that the ethyl alcohol is fully contacted with the crystal, and standing for 5min;
(5) And (3) rapidly filtering the sodium stannate crystal after three times of washing, and drying at the constant temperature for 2 hours, wherein the vacuum degree is-0.1 MPa and the temperature is 60 ℃.
The weighed sodium stannate product has the mass of 43.9kg, the chloride ion content is detected to be 0.007%, and the washing liquid is recycled.
Example 4
This example is a further example of the method for reducing chloride ion content in sodium stannate production process according to the present invention, comprising the steps of:
(1) Placing 50kg of sodium stannate initial product with 90% of crystal volume and 0.48% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Primary washing: pouring 4kg of glycerol and 6kg of water into a cleaning tank, performing ultrasonic treatment at 100W power for 5min, and immediately discharging the cleaning solution;
(3) And (3) secondary washing: pouring 6kg of absolute ethyl alcohol and 4kg of water into a cleaning tank, performing ultrasonic treatment for 5min at 240W power, and immediately discharging the cleaning solution;
(4) Three times of washing: pouring 20kg of absolute ethyl alcohol directly into a cleaning tank, performing ultrasonic treatment for 10min at 300W power to ensure that the absolute ethyl alcohol is fully contacted with the crystal, and standing for 5min;
(5) And (3) rapidly filtering the sodium stannate crystal after three times of washing, and drying at the constant temperature for 2 hours, wherein the vacuum degree is-0.1 MPa and the temperature is 90 ℃.
The weighed sodium stannate product has the mass of 43.4kg, the chloride ion content is detected to be 0.009%, and the washing liquid is recycled.
Comparative example 1
(1) Placing 50kg of a sodium stannate initial product with 90% of crystal volume and 0.37% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Washing with water for three times, adding 10kg of water each time, and putting out washing liquid after ultrasonic treatment with power of 240W for 5min;
(3) The weighed sodium stannate product has a mass of 41.9kg and a chloride ion content of 0.22% is detected.
Comparative example 2
(1) Placing 50kg of sodium stannate initial product with 90% of crystal volume and 0.38% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Primary washing: pouring 5kg of absolute ethyl alcohol and 5kg of water into a cleaning tank, performing ultrasonic treatment for 2min at 240W power, and immediately discharging the cleaning solution;
(3) And (3) secondary washing: pouring 5kg of absolute ethyl alcohol and 5kg of water into a cleaning tank, performing ultrasonic treatment for 2min at 240W power, and immediately discharging the cleaning solution;
(4) Three times of washing: pouring 20kg of absolute ethyl alcohol directly into a cleaning tank, performing ultrasonic treatment for 8min at 300W power to ensure that the ethyl alcohol is fully contacted with the crystal, and standing for 5min;
(5) And (3) rapidly filtering the sodium stannate crystal after three times of washing, and drying at the constant temperature of 80 ℃ for 1h under the vacuum degree of-0.1 MPa.
The weighed sodium stannate product has the mass of 44.0kg, the chloride ion content is detected to be 0.09%, and the washing liquid is recycled.
Comparative example 3
(1) Placing 50kg of sodium stannate initial product with 90% of crystal volume and 0.38% of chloride ion mass fraction into an ultrasonic cleaning tank;
(2) Primary washing: pouring 1kg of glycerol and 9kg of water into a cleaning tank, performing ultrasonic treatment at 240W for 2min, and immediately discharging the cleaning solution;
the weighed sodium stannate product has the mass of 45.1kg, the chloride ion content is detected to be 0.12%, and the washing liquid is recycled.
According to the comparison case, the mixed solvent of glycerol, water and ethanol can obviously remove chloride ions in sodium stannate products, and the mixed solvent is washed by single water, so that on one hand, more sodium stannate is lost, the washing effect is poor, and the experimental result shows that the method used by the invention is simple, effective, safe and environment-friendly.
The above embodiments are merely specific examples for further detailed description of the object, technical solution and advantageous effects of the present invention, and the present invention is not limited thereto. Any modification, equivalent replacement, improvement, etc. made within the scope of the present disclosure are included in the scope of the present invention.
Claims (6)
1. A method for reducing chloride ion content in sodium stannate production process, which is characterized by comprising the following steps:
(1) Placing a sodium stannate initial product with chloride ion content less than 1% into an ultrasonic cleaning tank;
(2) Primary washing: preparing glycerol and water into a washing liquid according to the mass ratio of 10% -40%, pouring the washing liquid into a washing tank, ultrasonically washing for 2-5min, and then discharging the washing liquid;
(3) And (3) secondary washing: preparing washing liquid from absolute ethyl alcohol and water according to the mass ratio of 40% -60%, pouring the washing liquid into a cleaning tank, ultrasonically cleaning for 2-5min, and then discharging the washing liquid;
(4) Three times of washing: directly pouring absolute ethyl alcohol into a cleaning tank, ultrasonically cleaning for 5-10min, and standing;
(5) Filtering and drying: and rapidly filtering the sodium stannate after three times of washing, transferring the sodium stannate into a vacuum drying oven, keeping the temperature at 60-90 ℃ for 1-2 hours, and drying to obtain a sodium stannate product with the chloride ion content less than 0.01%.
2. The method according to claim 1, characterized in that: in the step (1), the volume of crystals of the sodium stannate primary product accounts for 80-90% of the total volume, and the chloride ion content is less than 1%.
3. The method according to claim 1, characterized in that: the ultrasonic power of the ultrasonic washing in the step (2) and the ultrasonic washing in the step (3) is 100-240W.
4. The method according to claim 1, characterized in that: the ultrasonic power of the ultrasonic washing in the step (4) is 240-300W.
5. The method according to claim 1, characterized in that: and (3) in the step (5), drying in a vacuum drying oven, wherein the vacuum degree is-0.1 MPa.
6. The method according to claim 1, characterized in that: and (3) in the step (5), drying in a vacuum drying oven at 75-85 ℃.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| NL164833C (en) * | 1968-10-02 | 1981-02-16 | Goldschmidt Ag Th | METHOD FOR PREPARING SOLID SODIUM STANATE |
| JP4276322B2 (en) * | 1999-02-08 | 2009-06-10 | 日本化学産業株式会社 | Method for producing high purity alkali stannate compound |
| CN104818387B (en) * | 2015-04-22 | 2017-03-29 | 南昌航空大学 | A kind of method of sodium salt in separating-purifying arsenic alkaline slag |
| CN105481003A (en) * | 2015-11-23 | 2016-04-13 | 柳州华锡铟锡材料有限公司 | Method for reducing content of chloride ions in sodium stannate by using ultrasonic waves |
| CN105948104A (en) * | 2016-04-28 | 2016-09-21 | 中南大学 | Method for preparing sodium stannate by using tin anode slime oxygen pressure alkaline leaching |
| CN109134287B (en) * | 2018-08-27 | 2021-06-15 | 山东祥维斯生物科技股份有限公司 | Purification method of byproduct sodium chloride in betaine or betaine hydrochloride production |
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