CN103172109B - Method for preparing sodium stannate by utilizing tin-removed wastewater - Google Patents
Method for preparing sodium stannate by utilizing tin-removed wastewater Download PDFInfo
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- CN103172109B CN103172109B CN201310079993.1A CN201310079993A CN103172109B CN 103172109 B CN103172109 B CN 103172109B CN 201310079993 A CN201310079993 A CN 201310079993A CN 103172109 B CN103172109 B CN 103172109B
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Abstract
The invention relates to the sewage treatment technology and in particular relates to a method for preparing sodium stannate by utilizing tin-removed wastewater. The method for preparing sodium stannate by utilizing tin-removed wastewater comprises the following steps of: uniformly mixing tin paste, strong base and water to form a blank material; controlling the temperature to 90 DEG C to 600 DEG C, sintering the blank material for 2-4 hours and forming dry materials after cooling and crushing the blank material; mixing the dry materials with water to form first lixivium, stirring and reacting the first lixivium; carrying out solid-liquid separation on the first lixivium to obtain first filtrate and first sediment; evaporating, concentrating, crystallizing and cleaning the first filtrate to obtain a sodium stannate crude product; and drying the sodium stannate crude product to obtain the sodium stannate product. According to the method for preparing sodium stannate by utilizing tin-removed wastewater disclosed by the invention, the gentle preparation conditions are utilized for greatly reducing the roasting temperature of the existing process, greatly reducing the energy consumption and simplifying the leaching process. Moreover, the thin leaching rate is improved, the economic benefits are remarkable and the development prospect is good.
Description
Technical field
The present invention relates to sewage disposal technology, especially to the process of circuit board tin-stripping wastewater and the method for recycling.
Background technology
In circuit board machining process flow process, the etching operation of wiring board is an important step of wiring board processing, needs effectively to protect circuit before etching.The etching of wiring board divides acid etching and alkali etching two kinds of techniques, and acid etching adopts ink protection, and alkali etching adopts tin layers protection.Protection tin layers is needed to return after wiring board alkali etching.General tin stripping liquid is nitric acid liquid, is furnished with iron nitrate, nitric acid stablizer, copper inhibitor.When the tin amount in tin stripping liquid reaches finite concentration, move back tin ability and decline, thus scrap, produce tin-stripping wastewater.This type of tin-stripping wastewater, based on stanniferous, separately containing the contents of many kinds of heavy metal ion such as copper, iron, has complicated components, and change of water quality is large, pollution index high, must carry out the comprehensive regulation.
Due to each circuit board plant use move back tin or tin plating technique and method for recovering waste liquid is different, make tin-stripping wastewater complicated component, and component fluctuation is very large.According to current investigation and analysis, tin-stripping wastewater can be divided into following three kinds:
The first is the tin-stripping wastewater I containing more solid sediment, and this kind of throw out is white, and main component is cassiterite (SnO
2), supernatant liquor is the green solution containing a small amount of copper, but this tin-stripping wastewater storage is little.
The second is green muddy tin-stripping wastewater II.The feature of this kind of tin-stripping wastewater II be solution itself without obvious solid sediment, solution is thickness comparatively, and in colloidal sol shape, proportion is 1.42 ~ 1.48g/cm
3, can through ordinary filter paper, only leave a small amount of sticky shape foreign material at its surface, this tin-stripping wastewater accounts for about 85%.Comparison of ingredients is complicated, and mainly containing metallic elements such as Sn, Cu, Fe, Pb, its main component as shown in Table-1.
Table-1 tin-stripping wastewater II main component
| Composition | Sn | Cu | Pb | Fe |
| g/L | 50～150 | 30～50 | 40～60 | 10～40 |
Table-2 tin-stripping wastewater III supernatant liquor main components
| Composition | Sn | Cu | Pb | Fe | Ni |
| g/L | 0.10～1.00 | 1.00～10.00 | 0.001～0.100 | 0.001～0.020 | 0.001～0.010 |
The third is the tin-stripping wastewater III after long-term storage natural sedimentation, has a small amount of white cassiterite precipitation (SnO bottom it
2), supernatant liquor is main cupric by analysis, and other component content is less, and its composition is as shown in table-2.
The situation analyzing above-mentioned three kinds of tin-stripping wastewaters can be found out, tin-stripping wastewater I and tin-stripping wastewater III foreign matter content few, main component is comparatively single, be relatively easy to process.And tin-stripping wastewater II complicated component, several metal has certain content, and has higher reclamation value.Tin-stripping wastewater II is the maximum but one that output is the highest of intractability in similar waste water.
Current, ammonification or the process of bicarbonate of ammonia neutralisation are generally taked to tin-stripping wastewater, tin, iron, copper in tin-stripping wastewater are precipitated and forms tin mud.This tin mud sells relevant little smeltery process as the raw material of reduction tin metallurgy.There is serious drawback in this treatment process, the alkaline residue on the one hand after precipitation is as the raw material of pyrometallurgical smelting, and valuable metal recovery utilization ratio is lower, and waste is serious, also there is the risk of serious secondary pollution.
Also have maturing temperature higher (up to 850 ~ 950 DEG C) in the technique of some process tin-stripping wastewaters, in the reaction times longer (2.5 ~ 5 hours), greatly will certainly increase energy consumption, not only increase cost, also be unfavorable for environment protection.
Therefore, for the character feature of circuit board tin-stripping wastewater, overcome the many disadvantages that existing processing mode exists, find a kind of high efficiente callback and utilize its valuable metal and the method making it innoxious has important practical significance.
Summary of the invention
In order to solve the problem, the invention provides a kind of method utilizing tin-stripping wastewater to prepare sodium stannate, the defect of existing tin-stripping wastewater treatment process can be overcome, Simplified flowsheet, significantly reduce energy consumption, reduced cost, preferably quality product can also be obtained, obtain remarkable benefit.
This method utilizing tin-stripping wastewater to prepare sodium stannate, comprises the steps:
I, the heavy mud of described tin-stripping wastewater solid-liquid separation gained is dried, obtain raw material tin mud;
II, described tin mud is mixed with highly basic, water be mixed to form blank; Wherein, described tin atom is 1:4 ~ 10 with the ratio of the amount of substance of hydroxide ion, and the consumption of described water at least can dissolve described highly basic completely;
III, control temperature 90 ~ 600 DEG C, blank described in roasting 2 ~ 4 hours, forms siccative after cooling crush;
IV, be that described siccative and water are mixed to form the first leach liquor by 1:3 ~ 8 according to mass ratio, between control temperature 40 ~ 95 DEG C, stirring reaction 1 ~ 6 hour, then carries out solid-liquid separation to described first leach liquor and obtains the first filtrate and the first sediment;
V, described first filtrate evaporated, concentrate, crystallization; Sodium stannate crude product is obtained after cleaning described crystallization with strong base solution again;
VI, at temperature 100 ~ 110 DEG C, heat described sodium stannate crude product 2 ~ 3 hours, obtain sodium stannate product.
Preferably, also comprise baking operation in described step III, concrete operations are first control temperature is dry described blank in 60 ~ 130 DEG C, 0.5 ~ 1.5 hour, and then is progressively increased to 90 ~ 600 DEG C.
Preferably, the practical range that described maturing temperature is better is 90 ~ 500 DEG C.Low-temperature bake technique, significantly can reduce energy consumption.
Preferably, described tin atom is 1:5 with the ratio of the amount of substance of hydroxide ion.
Preferably, in described step II, the mass ratio of tin mud and water is 1:0.5 ~ 1.In this operation, adding of water is convenient to highly basic and tin mud energy Homogeneous phase mixing, can meet the water consumption of this object.Add water too much unsuitable, otherwise the temperature and time of subsequent step oven dry and roasting can be increased, be unfavorable for controlling energy consumption.
Preferably, in described step IV, the mass ratio of siccative and water is 1:5.
Preferably, described step IV also comprises secondary and leaches operation: be that 1:2 ~ 12 make described first sediment mix with water according to mass ratio, stirring reaction carried out solid-liquid separation after 1 ~ 6 hour.Secondary leaching operation is the recovery for metallic compound and alkali lye, is conducive to the recycling of environment protection and resource.
Preferably, add deslagging agent to before described first leach liquor solid-liquid separation, continue stirring 0.5 ~ 2 hour, described deslagging agent and the first leach liquor volume ratio are 1 ~ 20:1000.Adding of deslagging agent is to remove the metal ion such as copper, iron.
Wherein, described deslagging agent raw material is generally water miscible sulfide, conventional to be mass concentration be 2 ~ 10% sodium sulphite or ammonium sulfide solution.
Wherein, in described first filtrate, also add enough oxygenants, for removing excessive or residual deslagging agent.
Wherein, described oxygenant is hydrogen peroxide; Described highly basic is sodium hydroxide; The mass concentration of described step V strong base solution is 10 ~ 20%.
Beneficial effect: the present invention utilizes tin-stripping wastewater to prepare the sodium stannate product of technical grade, preparation condition is gentle, greatly reduces the maturing temperature of existing technique, significantly reduces energy consumption, and effective reduced cost effectively reduces the pollution to environment simultaneously; Technique is simply controlled, simplifies leaching flow process, and improves the leaching yield of tin.The present invention obtains product and all can be up to state standards, and has significant economic benefit and good development prospect.
Accompanying drawing explanation
Accompanying drawing is that the present invention utilizes tin-stripping wastewater to prepare the process flow sheet of sodium stannate.
Embodiment
Production method of the present invention mainly will precipitate the tin mud of formation from tin-stripping wastewater, mix at a certain temperature with alkaline solution, through operations such as leaching, slagging-off, condensing crystal, protection oven dry, and obtained technical grade sodium stannate (Na
2snO
33H
2o).
Embodiment 1
As shown in the figure, this method utilizing tin-stripping wastewater to prepare sodium stannate, comprises the steps:
I, described tin-stripping wastewater is carried out precipitation process, the heavy mud after filtration is at about 120 DEG C heating, dryings.This step can affect follow-up reaction mass, so must ensure heavy mud finish-drying.Heavy mud after oven dry is the tin mud as reaction raw materials, is ground into powdery for subsequent use with pulverizer.This heavy mud or tin argillization results of elemental analyses are as table 1.
Table 1 sinks mud/tin argillization results of elemental analyses
| Detection | Sn | Pb | Cu | Fe | As | Sb | Organism | Moisture * |
| Component content/% | 40.6 | 0.00013 | 4.11 | 6.93 | 0.00024 | 0.000201 | 0.48 | 49.0 |
(* is heavy mud detected result except " moisture ", and other detection is the detected result of tin mud)
II, the tin mud after pulverizing is mixed into blank with highly basic, water in mixing tank.
The present embodiment gets 100g tin mud, water 50g, is 1:5 according to tin atom and the ratio of the amount of substance of hydroxide ion, and the add-on calculating solid-state highly basic sodium hydroxide is about 68g.First be dissolved in the water completely by sodium hydroxide, then in this sodium hydroxide solution, add tin mud, stirring and evenly mixing forms the blank treating roasting.
III, also blank described in roasting is dried.
Above-mentioned blank is placed in stoving oven, drying program is set.First control about 100 DEG C to be drained by the moisture in described blank, process is about 1 hour; Then control temperature is increased to 300 DEG C, roasting 2 ~ 3 hours, impels tin mud and highly basic fully to react.After roasting completes, it is for subsequent use that cooling crush forms siccative.
IV, Na is leached
2snO
3.
Being transferred in batch extractor by described siccative, is that described siccative mixes with water by 1:5 according to mass ratio, and control extraction temperature 60 DEG C, stirring reaction 3 hours, obtains the first leach liquor.At leaching process coda, in order to remove the foreign ion such as cupric ion, iron ion, in the first leach liquor, be added into appropriate deslagging agent, insulated and stirred 1 hour.The present embodiment deslagging agent is the sodium sulfide solution of mass concentration 5%, and addition is that often liter of first leach liquor adds 10ml deslagging agent.
The first leach liquor after slagging-off is filtered, obtains the first filtrate and the first sediment.In gained first filtrate, the leaching yield of tin can reach more than 90%, the results are shown in Table 2.
The content of tin and tin leaching yield in table 2 first leach liquor, the first sediment
In addition, owing to also containing more metal values element in the first sediment, as copper, iron etc., the recyclable recycling of suitable processing is carried out to it.Clean the first sediment by suitable quantity of water in the present embodiment, scavenging solution can be back to the dissolving for solid-state highly basic in step II.Then secondary leaching can be carried out to the first sediment, for the recycling of metallic compound and alkali lye.
This secondary leaching process is: the mass ratio adjusting the first sediment and water is 1:2 ~ 12; Stirring reaction 1 ~ 6 hour, obtains the second leach liquor.To described second leach liquor solid-liquid separation, after filtering, gained the 3rd filtrate can be back to the dissolving for solid-state highly basic in step II; Gained the 3rd filter residue alkali content is extremely low, the elements such as main cupric, iron, and recyclable workshop is used for the raw materials of associated metal compound.
V, sodium stannate crude product is obtained.
First filtrate is transferred to evaporating pot, in the first filtrate, adds the deslagging agent oxidation removal that appropriate oxygenant makes to remain.The oxygenant of the present embodiment is industrial hydrogen peroxide, residual sulfide-oxidation can be removed.Then heating makes described first filtrate evaporation, treat its concentrated solution to stoste volume two/for the moment, filter, obtain sodium stannate crystallisate and mother liquor thereof.Sodium stannate crystallisate cleans with the sodium hydroxide solution of 10 ~ 20% again, obtains sodium stannate crude product.Disposing mother liquor is to mixing jar.
Table 3 technical grade sodium stannate Product checking analytical results
| Test item | Sn | Cu | Fe | NaOH | As | Pb | Sb | Insolubles |
| Component content/% | 38.21 | 0.00289 | 0.00272 | 1.31 | 0.000053 | 0.000031 | 0.00013 | 0.0078 |
VI, last, sodium stannate crude product described in vacuum-drying 2 ~ 3 hours at control temperature 100 ~ 110 DEG C, pulverizes, packs, and obtains technical grade sodium stannate product (Na
2snO
33H
2o).Wherein, as shown in table 3 below to the detection analytical results of sodium stannate product:
As can be seen from upper data, the sodium stannate product that the present invention produces meets technical grade product requirement.
For showing present invention process better, the present invention also provides the embodiment of different sinter process, and the sodium stannate product property contrast that these embodiments obtain.Embodiment 2, embodiment 3, embodiment 4 and embodiment 5 is the oven dry of step III, the adjustment of sinter process parameter with the difference of embodiment 1.Tin leaching yield various sodium stannate Product checking analytical results is to such as shown in table 4, table 5:
The tin leaching yield contrast of the different embodiment of table 4
Table 5: the sodium stannate Product checking analytical results contrast of different embodiment
From table 4, table 5, at maturing temperature 90 ~ 500 DEG C, roasting time 2 ~ 3h, all can obtain the tin leaching yield of more than 90%, and sodium stannate quality product all can be up to state standards.And in actual applications, maturing temperature can also be increased to 600 DEG C, namely control all can reach preferably implementation result within the scope of 90 ~ 600 DEG C.
Embodiment 1 is only the citing of more excellent processing step, it will be recognized by those skilled in the art that processing parameter can adjust to some extent in a proper range in actual applications, to adapt to the requirement of suitability for industrialized production.Such as, can be controlled within the scope of 100 ~ 130 DEG C to the oven dry of tin mud, ensure that moisture is thoroughly drained.Tin atom controls in the scope of 1:4 ~ 10 with the ratio of the amount of substance of hydroxide ion, the excessive leaching that effectively can promote tin of alkali lye, but also unnecessary consumption causes waste too greatly; Add water during tin mud mixes with highly basic, be in order to allow highly basic mix evenly, therefore can ensure that highly basic dissolves completely, the mass ratio of general control tin mud and water is 1:0.5 ~ 1.Siccative after roasting mixes with water and leaches, and the mass ratio of siccative and water can be 1:3 ~ 8, and extraction temperature can be controlled between 40 ~ 95 DEG C.In addition, the deslagging agent added in leaching process can select water miscible sulfide solution, and as ammonium sulfide or sodium sulfide solution, it is good that the mass concentration of deslagging agent controls 2% ~ 10%; General consumption can add according to the volume ratio 1 ~ 20:1000 of deslagging agent and leach liquor.
The present invention utilizes tin-stripping wastewater to prepare the sodium stannate product of technical grade, and preparation condition is gentle, greatly reduces the maturing temperature of existing technique, significantly reduces energy consumption, and effective reduced cost effectively reduces the pollution to environment simultaneously; Technique is simply controlled, simplifies leaching flow process; And improve the leaching yield of tin, effectively optimize quality product.The present invention is beneficial to the recycling of resource, has significant economic benefit, also realizes the Chemical Manufacture theory of green low-carbon simultaneously, meets the requirement of market development.
Claims (6)
1. utilize tin-stripping wastewater to prepare a method for sodium stannate, comprise the steps:
I, the heavy mud of described tin-stripping wastewater solid-liquid separation gained is dried, obtain raw material tin mud;
II, described tin mud is mixed with highly basic, water be mixed to form blank; Wherein, described tin atom is 1:4 ~ 10 with the ratio of the amount of substance of hydroxide ion, and the consumption of described water at least can dissolve described highly basic completely;
III, control temperature 90 ~ 500 DEG C, blank described in roasting 2 ~ 4 hours, forms siccative after cooling crush;
IV, be that described siccative and water are mixed to form the first leach liquor by 1:3 ~ 8 according to mass ratio, between control temperature 40 ~ 95 DEG C, stirring reaction 1 ~ 6 hour, then carries out solid-liquid separation to described first leach liquor and obtains the first filtrate and the first sediment;
V, described first filtrate evaporated, concentrate, crystallization; Sodium stannate crude product is obtained after cleaning described crystallization with strong base solution again;
VI, at temperature 100 ~ 110 DEG C, heat described sodium stannate crude product 2 ~ 3 hours, obtain sodium stannate product;
Described highly basic is sodium hydroxide;
Wherein, before described step III, first control temperature is dry described blank in 60 ~ 130 DEG C, 0.5 ~ 1.5 hour; In described step II, the mass ratio of tin mud and water is 1:0.5 ~ 1; Add deslagging agent to before described first leach liquor solid-liquid separation, continue stirring 0.5 ~ 2 hour, described deslagging agent and the first leach liquor volume ratio are 1 ~ 20:1000, while deslagging agent to be mass concentration be 2 ~ 10% sodium sulphite or ammonium sulfide solution.
2. prepare the method for sodium stannate according to claim 1, it is characterized in that, described tin atom is 1:5 with the ratio of the amount of substance of hydroxide ion.
3. according to claim 1 or 2, prepare the method for sodium stannate, it is characterized in that, in described step IV, the mass ratio of siccative and water is 1:5.
4. prepare the method for sodium stannate according to claim 1, it is characterized in that, described step IV also comprises secondary and leaches operation: be that 1:2 ~ 12 make described first sediment mix with water according to mass ratio, stirring reaction carried out solid-liquid separation after 1 ~ 6 hour.
5. prepare the method for sodium stannate according to claim 1, it is characterized in that, in described first filtrate, also add enough oxygenants, for removing excessive deslagging agent.
6. prepare the method for sodium stannate according to claim 1, it is characterized in that, described oxygenant is hydrogen peroxide; The mass concentration of described step V strong base solution is 10 ~ 20%.
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| NL164833C (en) * | 1968-10-02 | 1981-02-16 | Goldschmidt Ag Th | METHOD FOR PREPARING SOLID SODIUM STANATE |
| CN101497458B (en) * | 2008-01-30 | 2010-10-06 | 深圳市东江环保股份有限公司 | Method for preparing sodium stannate using circuit board tin-stripping wastewater |
| CN101532096B (en) * | 2009-04-01 | 2011-01-26 | 深圳市危险废物处理站有限公司 | A recovery method of tin in tin-stripping waste liquid |
| CN101984097A (en) * | 2010-11-24 | 2011-03-09 | 苏州市环境工程有限责任公司 | Method for comprehensive recovery of heavy metal from spent solder stripper |
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