CN102849787A - Preparation method of soluble alkali metal stannate - Google Patents
Preparation method of soluble alkali metal stannate Download PDFInfo
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- CN102849787A CN102849787A CN2012103132200A CN201210313220A CN102849787A CN 102849787 A CN102849787 A CN 102849787A CN 2012103132200 A CN2012103132200 A CN 2012103132200A CN 201210313220 A CN201210313220 A CN 201210313220A CN 102849787 A CN102849787 A CN 102849787A
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Abstract
The invention relates to a preparation method of a soluble alkali metal stannate, and belongs to the technical field of the inorganic chemical engineering. The preparation method comprises the following steps: 1, adding metallic stannum flowers to a glass reaction vessel, adding a hydrochloric acid solution by complete reaction, and completing a reaction at room temperature; 2, adding hydrogen peroxide to a solution formed in step 1 by complete reaction, and completing a reaction at 75-90DEG C; 3, adding ammonia water having an amount greater than a reaction amount to a solution formed in step 2 to neutralize until complete precipitation, and washing and filtering the resultant precipitate to obtain a stannic acid; and 4, reacting the stannic acid with an alkali solution at 30-80DEG C, and concentrating and drying to obtain the soluble alkali metal stannate. The preparation method has the advantages of simplicity, low cost, no use of toxic gases comprising chlorine or the like, no generation of harmful gases comprising nitrogen oxides or the like, environmental protection and the like, and can be applied in industrialized production.
Description
Technical field
The present invention relates to a kind of preparation method of soluble alkali metal stannate, belong to technical field of inorganic chemical industry.
Background technology
Soluble alkali metal stannate such as sodium stannate, potassium stannate etc. are important industrial chemicals, are widely used in the industrial circles such as plating, electronics, printing and dyeing industry, glass, pottery, coinage, automobile making, tinned food box, tight instrument.
At present the report of the relevant method that prepare sodium stannate or potassium stannate soluble alkali metal stannate is more, but the problems such as these methods all exist that energy consumption is high, employing toxic raw materials or complicated process of preparation.A kind of method of utilizing tin raw material direct production potassium stannate is disclosed such as patent documentation CN101544399A, being about to tin and tin alloy carries out chemical reaction with potassium hydroxide, saltpetre and makes granular thick potassium stannate under 300 ℃ to 600 ℃ temperature in reactor, then with the thick potassium stannate of water dissolution, refiningly purify, concentrated, separate, oven dry obtains product at last.The method temperature of reaction is higher, and energy consumption is large, needs simultaneously the follow-up steps such as refining purification, and preparation cost is high, and there are the shortcomings such as perishable in institute cylinder iron reactor under high temperature, highly basic condition.What patent documentation CN101544397 adopted is that the method similar to CN101544399A prepares sodium stannate.Patent CN1546383A provides a kind of preparation method of potassium stannate, adopt tin and concentrated nitric acid to generate β-stannic acid, again with β-stannic acid and potassium hydroxide heating congruent melting, cooling, be dissolved in water, filter evaporation concentration crystallization product potassium stannate, can produce a large amount of nitrous oxides exhaust gas in the method preparation process, be unfavorable for suitability for industrialized production.Patent documentation CN1078444 discloses a kind of preparation method of alkali metal stannate, as raw material take metallic tin, mixing acid direct and concentrated nitric acid and concentrated hydrochloric acid reacts, then reacted clear liquor is slow and strong aqua effect, the white precipitate that reaction obtains is dissolved in the alkaline solution fully, obtain alkali metal stannate through concentrated, crystallization, oven dry and pulverizing, the method still has the processing problem of poisonous gas oxynitride.Patent documentation CN1872699A discloses a kind of preparation method of potassium stannate, it adopts golden tin and chlorine reaction, synthetic tin tetrachloride, then alkali neutralization, through solid-liquid separation, obtain positive stannic acid, positive stannic acid synthesizes potassium stannate with potassium hydroxide again, after, the drying concentrated finally by pervaporation, obtain the potassium stannate product.The method has used the larger chlorine of toxicity as one of raw material, and there is larger potential safety hazard in production process.Patent CN101643237A document has adopted the method similar to CN1872699A to prepare sodium stannate.
Therefore, the above-mentioned existing existing problem of method for preparing the soluble alkali metal stannates such as sodium stannate or potassium stannate awaits studying new preparation method and is solved, thereby promotes the industrial applications of soluble alkali metal stannate.
Summary of the invention
The object of the invention is to overcome the problems such as existing preparation soluble alkali metal stannate cost is high, energy consumption is high, environmental pollution is serious, a kind of novel method for preparing the soluble alkali metal stannate is provided, have that preparation technology is simple, cost is low, advantages of environment protection.
The step that realizes the technical scheme that above-mentioned purpose of the present invention adopts is as follows:
1. the metallic tin flower is joined in the glass reaction still, by complete reaction adding hydrochloric acid soln, at room temperature finish reaction;
2. in the solution that 1. forms by complete reaction adding hydrogen peroxide, under 75～90 ℃, finish reaction;
3. add the ammonia neutralization greater than reacting weight in the solution that 2. forms, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid;
4. with stannic acid and alkaline solution 30～80 ℃ of reactions, again through concentrated, dry soluble alkali metal stannate.
The concentration of hydrochloric acid is 25～32wt% in the above-mentioned 1. step, and the mol ratio of hydrochloric acid and metallic tin flower is 3:1～5:1, and the reaction times is 2 ~ 7h.
Hydrogen peroxide concentration is 20～30wt% in the above-mentioned 2. step, and the mol ratio of hydrogen peroxide and metallic tin flower is 2:1～1:2, and the reaction times is 4～8h.
Alkaline solution is sodium hydroxide or potassium hydroxide solution in the above-mentioned 4. step, and the mol ratio of stannic acid and alkali is 1:2, and the reaction times is 4～8 h, reaction solution relative vacuum degree 0～-83KPa under concentrating under reduced pressure.
Compared with prior art, the present invention has following advantage: 1. take tin flower, hydrochloric acid, hydrogen peroxide, potassium hydroxide, sodium hydroxide etc. as raw material, and synthesizing soluble alkali metal stannate under the lesser temps normal pressure, the characteristics such as it is simple to have the preparation method, and energy consumption is low.2. preparation process is easy to control, and washings is easy to process, and sodium stannate, potassium stannate yield are higher.3. do not adopt the larger raw materials of hazardness such as chlorine, do not produce the toxic gases such as oxynitride in the production process, safe preparation process, environmental protection.
Embodiment
The invention will be further described with embodiment for the below.
Embodiment 1
500 g metallic tin flowers are joined in the glass reaction still, then are that 32% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 3:1.Then add concentration and be 20% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 2:1, after temperature of reaction is 85 ℃ of lower reaction 4h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 4 h under 30 ℃ with stannic acid and sodium hydroxide solution, wherein the mol ratio of stannic acid and sodium hydroxide is 1:2, obtains sodium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of sodium stannate is 52.4%.
Embodiment 2
500 g metallic tin flowers are joined in the glass reaction still, then are that 28% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 4:1.Then add concentration and be 25% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 1:1, after temperature of reaction is 85 ℃ of lower reaction 6 h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 5 h under 50 ℃ with stannic acid and sodium hydroxide solution, wherein the mol ratio of stannic acid and sodium hydroxide is 1:2, obtains sodium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of sodium stannate is 79.3%.
Embodiment 3
500 g metallic tin flowers are joined in the glass reaction still, then are that 32% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 4:1.Then add concentration and be 30% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 1:1, after temperature of reaction is 85 ℃ of lower reaction 7h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 6 h under 60 ℃ with stannic acid and sodium hydroxide solution, wherein the mol ratio of stannic acid and sodium hydroxide is 1:2, obtains sodium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of sodium stannate is 98.6%.
Embodiment 4
500 g metallic tin flowers are joined in the glass reaction still, then are that the hydrochloric acid of 30 % joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 5:1.Then add concentration and be 30% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 1:2, after temperature of reaction is 85 ℃ of lower reaction 8 h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 7 h under 80 ℃ with stannic acid and sodium hydroxide solution, wherein the mol ratio of stannic acid and sodium hydroxide is 1:2, obtains sodium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of sodium stannate is 79.9%.
Embodiment 5
500 g metallic tin flowers are joined in the glass reaction still, then are that 32% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 4:1.Then add concentration and be 30% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 1:1, after temperature of reaction is 85 ℃ of lower reaction 8h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 7 h under 70 ℃ with stannic acid and sodium hydroxide solution, wherein the mol ratio of stannic acid and sodium hydroxide is 1:2, obtains sodium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of sodium stannate is 99.4%.
Embodiment 6
500 g metallic tin flowers are joined in the glass reaction still, then are that 25% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 3:1.Then add concentration and be 20% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 2:1, after temperature of reaction is 85 ℃ of lower reaction 4h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 4 h under 30 ℃ with stannic acid and potassium hydroxide solution, wherein the mol ratio of stannic acid and potassium hydroxide is 1:2, obtains potassium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of potassium stannate is 64.9%.
Embodiment 7
500 g metallic tin flowers are joined in the glass reaction still, then are that 30% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 5:1.Then add concentration and be 28% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 1:2, after temperature of reaction is 85 ℃ of lower reaction 6 h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 7 h under 70 ℃ with stannic acid and potassium hydroxide solution, wherein the mol ratio of stannic acid and potassium hydroxide is 1:2, obtains potassium stannate soluble alkali metal stannate through concentrating under reduced pressure, drying again, the yield of potassium stannate is 74.2%.
Embodiment 8
500 g metallic tin flowers are joined in the glass reaction still, then are that 32% hydrochloric acid joins in the reactor with concentration, at room temperature react 2.0 h, and the mol ratio of hydrochloric acid and metallic tin flower is 4:1.Then add concentration and be 30% hydrogen peroxide, the mol ratio of hydrogen peroxide and metallic tin flower is 1:1, after temperature of reaction is 85 ℃ of lower reaction 8h, adds ammonia neutralization, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid.Reaction 7 h under 70 ℃ with stannic acid and potassium hydroxide solution, wherein the mol ratio of stannic acid and potassium hydroxide is 1:2, obtains sodium stannate soluble alkali metal potassium hydrochlorate through concentrating under reduced pressure, drying again, the yield of potassium stannate is 98.7%.
Claims (4)
1. the preparation method of a soluble alkali metal stannate is characterized in that processing step is as follows:
1. the metallic tin flower is joined in the glass reaction still, by complete reaction adding hydrochloric acid soln, at room temperature finish reaction;
2. in the solution that 1. forms by complete reaction adding hydrogen peroxide, under 75～90 ℃, finish reaction;
3. add the ammonia neutralization greater than reacting weight in the solution that 2. forms, until precipitation fully, the gained precipitation through washing, filter and obtain stannic acid;
4. with stannic acid and alkaline solution 30～80 ℃ of reactions, again through concentrated, dry soluble alkali metal stannate.
2. the preparation method of soluble alkali metal stannate according to claim 1, it is characterized in that: 1. the concentration of hydrochloric acid is 25～32wt% in the step, and the mol ratio of hydrochloric acid and metallic tin flower is 3:1～5:1, and the reaction times is 2 ~ 7h.
3. the preparation method of soluble alkali metal stannate according to claim 1, it is characterized in that: 2. hydrogen peroxide concentration is 20～30wt% in the step, and the mol ratio of hydrogen peroxide and metallic tin flower is 2:1～1:2, and the reaction times is 4～8h.
4. the preparation method of soluble alkali metal stannate according to claim 1, it is characterized in that: 4. alkaline solution is sodium hydroxide or potassium hydroxide solution in the step, the mol ratio of stannic acid and alkali is 1:2, reaction times is 4～8 h, reaction solution relative vacuum degree 0～-83KPa under concentrating under reduced pressure.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000226214A (en) * | 1999-02-08 | 2000-08-15 | Nihon Kagaku Sangyo Co Ltd | Production of high-purity alkali stannate compound |
| CN101643237A (en) * | 2009-06-22 | 2010-02-10 | 云南锡业集团（控股）有限责任公司 | Method for producing sodium stannate |
| CN102173448A (en) * | 2011-02-26 | 2011-09-07 | 西陇化工股份有限公司 | Method for preparing alkali metal stannate |
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- 2012-08-30 CN CN2012103132200A patent/CN102849787A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000226214A (en) * | 1999-02-08 | 2000-08-15 | Nihon Kagaku Sangyo Co Ltd | Production of high-purity alkali stannate compound |
| CN101643237A (en) * | 2009-06-22 | 2010-02-10 | 云南锡业集团（控股）有限责任公司 | Method for producing sodium stannate |
| CN102173448A (en) * | 2011-02-26 | 2011-09-07 | 西陇化工股份有限公司 | Method for preparing alkali metal stannate |
Non-Patent Citations (3)
| Title |
|---|
| 曾繁杰等: "无水四氯化锡的制备", 《化学通报》 * |
| 杜安等: "《金属表面着色技术》", 31 March 2012, 化学工业出版社 * |
| 郝润蓉等: "《无机化学丛书·第3卷，碳、硅、锗分族》", 31 March 2011, 科学出版社 * |
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Application publication date: 20130102 |