CN105366713B - A kind of method utilizing stannum waste residue to produce high-purity sodium stannate - Google Patents
A kind of method utilizing stannum waste residue to produce high-purity sodium stannate Download PDFInfo
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Abstract
The present invention relates to a kind of method utilizing stannum waste residue to produce high-purity sodium stannate, comprise the following steps: (1) stannum waste residue, water and hydrochloric acid are put in reactor, be slowly introducing chlorine, dissolve tin metal；(2) solution is transferred to Xi Huazhong, and reacting by heating prepares stannous chloride solution, removes arsenic, antimony, lead simultaneously；In solution alkali liquor and synthesis stannous hydroxide；(4) stannous hydroxide is added synthesis sodium stannite solution in sodium hydroxide solution；(5) in sodium stannite solution, it is slowly added to hydrogen peroxide, obtains sodium stannate solution, remove ferrum simultaneously；(6) solution is through condensing crystallizing, filtration, dried, obtains sodium stannate product.The method process condition of the present invention is gentle, and energy consumption is low, the sodium stannate prepared and content summation >=99.95% of sodium hydroxide.Under acid condition, remove the impurity such as arsenic, antimony, lead by stannum reducing process, make three kinds of impurity content summation≤0.0030% in sodium stannate product.Iron impurity in the basic conditions, makes iron content≤0.0015% in sodium stannate product.
Description
Technical field
The invention belongs to the production field of sodium stannate, be related specifically to a kind of method utilizing stannum waste residue to produce high-purity sodium stannate.
Background technology
Sodium stannate, colourless hexagonal plate crystal or white powder, tasteless, it is insoluble in Organic substance, soluble in water, aqueous solution is alkalescence.It is mainly used in electroplating industry alkaline tin plating and copper facing, and the plating of the alloy such as ashbury metal, Zinc-tin alloy, aluminium alloy and chemical plating；It is used as fireproof agent, weighting agent in textile industry；It is used as mordant etc. at dyeing.
The production method of sodium stannate mainly has three kinds:
(1) oxidant alkaline hydrolysis: describe a kind of method that alkaline hydrolysis produces sodium stannate in Chinese patent CN200710050721.3, stannum material is thick sodium stannate with caustic soda, the miscible synthetic reaction of sodium nitrate, then nitrate anion is decomposed in high-temperature calcination, by leaching, purification and impurity removal, concentration, centrifugation, dry, pulverizing, prepare sodium stannate product.
(2) direct fusion method: mention in Chinese patent CN85104036, by Tin concentrate with sodium hydroxide in 400～500 DEG C of congruent meltings 2～3h, then through leaching, purifies the impurity such as arsenic removal, antimony, lead, silicon, concentrates, centrifugation, prepared sodium stannate product after drying.
(3) method prepared by butter of tin: Chinese patent CN101643237A proposes a kind of method that sodium stannate prepared by butter of tin, butter of tin neutralizes with alkali, the precipitation obtained is through adding water washing, solid-liquid separation, obtain positive stannic acid, positive stannic acid synthesizes sodium stannate with sodium hydroxide, through condensing crystallizing, filter, be dried, pulverize after obtain sodium stannate product.
Shortcomings in the production method of above-mentioned three kinds of sodium stannates: 1. in oxidant alkaline hydrolysis, pyrolytic nitrate anion, the time is long, and energy consumption is high, and nitrate anion, lead, antimony, arsenic impurities content are high, remove impurity difficulty under the conditions of alkalescence；2. directly fusion method, anaerobic agent, reaction conversion ratio is low, and pyroreaction energy consumption is big, and the impurity content such as arsenic, antimony, lead is high, it is difficult to removing, leach the quantity of slag produced bigger than the quantity of slag that direct fusion method produces, direct yield is low；3. method prepared by butter of tin, and intermediate products stannic hydroxide granule is thin, it is difficult to sedimentation washing dechlorination root.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of method utilizing stannum waste residue to produce high-purity sodium stannate, the inventive method process condition is gentle, and energy consumption is low, prepares sodium stannate purity high.
To achieve these goals, the present invention is achieved by the following technical solutions: a kind of method utilizing stannum waste residue to produce high-purity sodium stannate, comprises the steps:
(1) stannum dissolves: put in reactor by stannum waste residue, water and concentrated hydrochloric acid, is slowly introducing chlorine, dissolves tin metal；Stannum waste residue, water, the proportioning of concentrated hydrochloric acid be: stannum waste residue: water: concentrated hydrochloric acid=150～250g:100～200mL:10～20mL, when being passed through chlorine leach tin metal, when solution Baume degrees reaches 60～80Be, stops being passed through chlorine；
(2) reduce arsenic removal, antimony, lead: solution step (1) obtained is transferred to Xi Huazhong, stannum flower: solution=100～2 00g:100～250mL, 60～100 DEG C of reacting by heating 2～6h, after reacting liquid filtering, sedimentation, i.e. obtain stannous chloride solution, remove arsenic, antimony, lead in the process；
(3) synthesizing stannous hydroxide: solution step (2) obtained slowly neutralizes with alkali liquor under agitation, controlling reaction temperature is 40 DEG C～60 DEG C, and reaction end pH value is 5～8, and precipitation dries by centrifugation, wash dechlorination root obtains stannous hydroxide；
(4) synthesize sodium stannite: (3) step slowly obtaining stannous hydroxide under agitation and adds in sodium hydroxide solution, reaction temperature is 30～80 DEG C, and reaction end pH value is 8～10, obtains sodium stannite solution；
(5) synthesize sodium stannate: at 60～90 DEG C in sodium stannite solution step (4) obtained, under conditions of being stirred continuously, it is slowly added to hydrogen peroxide, until solution is gradually converted into light yellow transparent solution by furvous, solution is after sedimentation, filtering, i.e. obtain sodium stannate solution, ferrum can be removed in the process；
(6) post processing: (5) step obtains solution through condensing crystallizing, filtration, dried, obtains sodium stannate product.
Described stannum waste residue be stannum smelt or stannum processing produce slag in one or more, including with stannum be raw material electrolysis produce stannous sulfate produce the earth of positive pole, stannum pole plate casting time produce pot face oxidizing slag, with stannum be the pot face oxidizing slag that raw material production alloy produces, the pot face oxidizing slag produced for raw material production solder with stannum and production glass putty time generation oversize.
The most described alkali liquor of step is one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, and concentration is 15～25%.
The most described concentration of sodium hydroxide solution of step is 20～25%.
It is 5～10mL/min that step (5) hydrogen peroxide adds speed, and mixing speed is 30～70r/min.
Described concentrated hydrochloric acid refers to the hydrochloric acid that mass fraction is 36-38%.
The whole processing step of the present invention is as shown in following chemical equation:
Reduction arsenic removal, antimony, lead, ferrum principle are as shown in following chemical equation:
Compared with prior art, the invention has the beneficial effects as follows:
1. the method process condition of the present invention is gentle, and energy consumption is low, the sodium stannate prepared and content summation >=99.95% of sodium hydroxide.
2. the method process condition of the present invention is gentle, and reaction temperature is all less than 100 DEG C.
3. the present invention is in stannous chloride preparation process, under acid condition, removes the impurity such as arsenic, antimony, lead by stannum reducing process, makes three kinds of impurity content summation≤0.0030% in sodium stannate product.
4. the present invention is during sodium stannite synthesis sodium stannate, and iron impurity under the conditions of alkalescence makes iron content≤0.0015% in sodium stannate product.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to the scope that embodiment represents.
Embodiment
1
:
It is that 36-38% concentrated hydrochloric acid is put in reactor by 150g stannum waste residue (producing, for raw material electrolysis, the earth of positive pole that stannous sulfate produces with stannum), 100mL water and 10mL mass fraction, it is slowly introducing chlorine leach tin metal, stops when solution Baume degrees is 60Be being passed through chlorine.100mL solution is transferred to during 100g stannum spends, 60 DEG C of reacting by heating 3h, after reacting liquid filtering, sedimentation, i.e. obtains stannous chloride solution.Solution the most slowly with 15% sodium carbonate liquor neutralize, control reaction temperature be 50 DEG C, reaction end pH value is 5, precipitation dry by centrifugation, wash dechlorination root obtain stannous hydroxide.Slowly adding in 20% sodium hydroxide solution by stannous hydroxide under agitation, reaction temperature is 80 DEG C, and reaction end pH value is 10.Then at 80 DEG C, being stirred continuously down, be slowly added to hydrogen peroxide in sodium stannite solution, until solution is gradually converted into light yellow transparent solution by furvous, solution, after sedimentation, filtering, i.e. obtains sodium stannate solution.Solution is through condensing crystallizing, filtration, dried, and the content summation obtaining 250.5g product, sodium stannate and sodium hydroxide is 99.95%, and arsenic, antimony, three kinds of impurity mass content summations of lead are 0.0027%, and weight of iron content is 0.0012%.
Embodiment
2
:
It is that 36-38% concentrated hydrochloric acid is put in reactor by 250g stannum waste residue (the pot face oxidizing slag produced during the casting of stannum pole plate), 150mL water and 15mL mass fraction, is slowly introducing chlorine leach tin metal, stops when solution Baume degrees is 65Be being passed through chlorine.150mL solution is transferred to during 150g stannum spends, 70 DEG C of reacting by heating 5h, after reacting liquid filtering, sedimentation, i.e. obtains stannous chloride solution.Solution the most slowly with 20%NaOH solution neutralize, control reaction temperature be 60 DEG C, reaction end pH value is 6, precipitation dry by centrifugation, wash dechlorination root obtain stannous hydroxide.Slowly adding in 21% sodium hydroxide solution by stannous hydroxide under agitation, reaction temperature is 70 DEG C, and reaction end pH value is 9.Then at 90 DEG C, being stirred continuously down, be slowly added to hydrogen peroxide in sodium stannite solution, until solution is gradually converted into light yellow transparent solution by furvous, solution, after sedimentation, filtering, i.e. obtains sodium stannate solution.Solution, through condensing crystallizing, filtration, dried, obtains the content summation 99.96% of 340.2g product, sodium stannate and sodium hydroxide, and arsenic, antimony, three kinds of impurity mass content summations of lead are 0.0022%, and weight of iron content is 0.0010%.
Embodiment
3
:
It is that 36-38% concentrated hydrochloric acid is put in reactor by 200g stannum waste residue (with stannum for pot face oxidizing slag that raw material production alloy produces), 200mL water and 15mL mass fraction, is slowly introducing chlorine leach tin metal, stop when solution Baume degrees is 70Be being passed through chlorine.200mL solution is transferred to during 200g stannum spends, 80 DEG C of reacting by heating 2h, after reacting liquid filtering, sedimentation, i.e. obtains stannous chloride solution.Solution the most slowly with 20%KOH solution neutralize, control reaction temperature be 40 DEG C, reaction end pH value is 7, precipitation dry by centrifugation, wash dechlorination root obtain stannous hydroxide.Slowly adding in 22% sodium hydroxide solution by stannous hydroxide under agitation, reaction temperature is 60 DEG C, and reaction end pH value is 8.Then at 80 DEG C, being stirred continuously down, be slowly added to hydrogen peroxide in sodium stannite solution, until solution is gradually converted into light yellow transparent solution by furvous, solution, after sedimentation, filtering, i.e. obtains sodium stannate solution.Solution, through condensing crystallizing, filtration, dried, obtains content summation >=99.95% of 313.8g product, sodium stannate and sodium hydroxide, and arsenic, antimony, three kinds of impurity mass content summations of lead are 0.0023%, and weight of iron content is 0.0012%.
Embodiment
4
:
It is that 36-38% concentrated hydrochloric acid is put in reactor by 200g stannum waste residue (with stannum for pot face oxidizing slag that raw material production solder produces), 150mL water and 20mL mass fraction, is slowly introducing chlorine leach tin metal, stop when solution Baume degrees is 75Be being passed through chlorine.150mL solution is transferred to during 100g stannum spends, 90 DEG C of reacting by heating 4h, after reacting liquid filtering, sedimentation, i.e. obtains stannous chloride solution.Solution the most slowly with 25% solution of potassium carbonate neutralize, control reaction temperature be 40 DEG C, reaction end pH value is 8, precipitation dry by centrifugation, wash dechlorination root obtain stannous hydroxide.Slowly adding in 23% sodium hydroxide solution by stannous hydroxide under agitation, reaction temperature is 50 DEG C, and reaction end pH value is 8.Then at 70 DEG C, being stirred continuously down, be slowly added to hydrogen peroxide in sodium stannite solution, until solution is gradually converted into light yellow transparent solution by furvous, solution, after sedimentation, filtering, i.e. obtains sodium stannate solution.Solution, through condensing crystallizing, filtration, dried, obtains content summation >=99.96% of 298.3g product, sodium stannate and sodium hydroxide, and arsenic, antimony, three kinds of impurity mass content summations of lead are 0.0019%, and weight of iron content is 0.0011%.
Embodiment
5
:
It is that 36-38% concentrated hydrochloric acid is put in reactor by 150g stannum waste residue (oversize produced when producing glass putty), 100mL water and 20mL mass fraction, is slowly introducing chlorine leach tin metal, stops when solution Baume degrees is 80Be being passed through chlorine.100mL solution is transferred to during 200g stannum spends, 100 DEG C of reacting by heating 6h, after reacting liquid filtering, sedimentation, i.e. obtains stannous chloride solution.Solution the most slowly with 15% sodium carbonate liquor neutralize, control reaction temperature be 40 DEG C, reaction end pH value is 7, precipitation dry by centrifugation, wash dechlorination root obtain stannous hydroxide.Slowly adding in 25% sodium hydroxide solution by stannous hydroxide under agitation, reaction temperature is 30 DEG C, and reaction end pH value is 9.Then at 60 DEG C, being stirred continuously down, be slowly added to hydrogen peroxide in sodium stannite solution, until solution is gradually converted into light yellow transparent solution by furvous, solution, after sedimentation, filtering, i.e. obtains sodium stannate solution.Solution, through condensing crystallizing, filtration, dried, obtains content summation >=99.96% of 230.1g product, sodium stannate and sodium hydroxide, and arsenic, antimony, three kinds of impurity mass content summations of lead are 0.0023%, and weight of iron content is 0.0014%.
Claims (6)
1. one kind utilizes the method that stannum waste residue produces high-purity sodium stannate, it is characterised in that comprise the steps:
(1) stannum dissolves: put in reactor by stannum waste residue, water and concentrated hydrochloric acid, is slowly introducing chlorine, dissolves tin metal；Stannum waste residue, water, the proportioning of concentrated hydrochloric acid be: stannum waste residue: water: concentrated hydrochloric acid=150～250g:100～200mL:10～20mL, when being passed through chlorine leach tin metal, when solution Baume degrees reaches 60～80 ° of B é, stops being passed through chlorine；
(2) reduce arsenic removal, antimony, lead: solution step (1) obtained is transferred to Xi Huazhong, stannum flower: solution=100～200g:100～250mL, 60～100 DEG C of reacting by heating 2～6h, after reacting liquid filtering, sedimentation, i.e. obtain stannous chloride solution, remove arsenic, antimony, lead in the process；
(3) synthesizing stannous hydroxide: solution step (2) obtained slowly neutralizes with alkali liquor under agitation, controlling reaction temperature is 40 DEG C～60 DEG C, and reaction end pH value is 5～8, and precipitation dries by centrifugation, wash dechlorination root obtains stannous hydroxide；
(4) synthesize sodium stannite: (3) step slowly obtaining stannous hydroxide under agitation and adds in sodium hydroxide solution, reaction temperature is 30～80 DEG C, and reaction end pH value is 8～10, obtains sodium stannite solution；
(5) synthesize sodium stannate: sodium stannite solution step (4) obtained, at 60～90 DEG C, under conditions of being stirred continuously, is slowly added to hydrogen peroxide, until solution is gradually converted into light yellow transparent solution by furvous, solution, after sedimentation, filtering, i.e. obtains sodium stannate solution, can remove ferrum in the process；
(6) post processing: (5) step obtains solution through condensing crystallizing, filtration, dried, obtains sodium stannate product.
The method utilizing stannum waste residue to produce high-purity sodium stannate the most according to claim 1, it is characterized in that: described stannum waste residue be stannum smelt or stannum processing produce slag in one or more, including with stannum be raw material electrolysis produce stannous sulfate produce the earth of positive pole, stannum pole plate casting time produce pot face oxidizing slag, with stannum be the pot face oxidizing slag that raw material production alloy produces, the pot face oxidizing slag produced for raw material production solder with stannum and production glass putty time generation oversize.
The method utilizing stannum waste residue to produce high-purity sodium stannate the most according to claim 1, it is characterised in that: the most described alkali liquor of step is one or more in sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, and concentration is 15～25%.
The method utilizing stannum waste residue to produce high-purity sodium stannate the most according to claim 1, it is characterised in that: the most described concentration of sodium hydroxide solution of step is 20～25%.
The method utilizing stannum waste residue to produce high-purity sodium stannate the most according to claim 1, it is characterised in that: it is 5～10mL/min that step (5) hydrogen peroxide adds speed, and mixing speed is 30～70r/min.
The method utilizing stannum waste residue to produce high-purity sodium stannate the most according to claim 1, it is characterised in that: described concentrated hydrochloric acid refers to the hydrochloric acid that mass fraction is 36-38%.
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| RU2717528C1 (en) * | 2019-11-22 | 2020-03-23 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Юго-Западный государственный университет" (ЮЗГУ) | Method of producing tin (ii) chloride by oxidising metal |
| CN110817940A (en) * | 2019-11-28 | 2020-02-21 | 云南锡业锡化工材料有限责任公司 | Method for preparing low free alkali and low water solution turbidity sodium stannate |
| CN111411242A (en) * | 2020-05-06 | 2020-07-14 | 云南锡业股份有限公司冶炼分公司 | Method for dechlorinating high-chlorine tin-containing material |
| CN114772631A (en) * | 2022-04-20 | 2022-07-22 | 柳州华锡有色设计研究院有限责任公司 | Method for deeply removing residual chlorine in ITO powder slurry by using ozone |
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| JPS575829A (en) * | 1980-06-14 | 1982-01-12 | Dowa Mining Co Ltd | Separating and recovering method for tin in lead refining process |
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| CN104032131A (en) * | 2013-06-27 | 2014-09-10 | 中石化上海工程有限公司 | Method for processing high-tin anode slurry |
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