CN103172109A - 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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- CN103172109A CN103172109A CN2013100799931A CN201310079993A CN103172109A CN 103172109 A CN103172109 A CN 103172109A CN 2013100799931 A CN2013100799931 A CN 2013100799931A CN 201310079993 A CN201310079993 A CN 201310079993A CN 103172109 A CN103172109 A CN 103172109A
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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 method for processing and the recycling of circuit board tin-stripping wastewater.
Background technology
In circuit board machining process flow process, the etching operation of wiring board is an important step of wiring board processing, needs before etching circuit is effectively protected.The etching of wiring board divides acid etching and two kinds of techniques of alkali etching, and the printing ink protection is adopted in acid etching, and alkali etching adopts the protection of tin layer.Need after the wiring board alkali etching protection tin layer is returned.General tin stripping liquid is nitric acid liquid, is furnished with iron nitrate, nitric acid stablizer, copper inhibitor.Tin amount in tin stripping liquid reaches finite concentration, moves back the tin ability and descends, thereby scrap, and produces tin-stripping wastewater.This type of tin-stripping wastewater separately contains the contents of many kinds of heavy metal ion such as copper, iron take stanniferous as main, has complicated components, and change of water quality is large, the pollution index high, must carry out the comprehensive regulation.
Due to each circuit board plant use to move back tin or tin plating technique and method for recovering waste liquid different, make the tin-stripping wastewater complicated component, and component fluctuation is very large.According to present investigation and analysis, tin-stripping wastewater can be divided into following three kinds:
The first is the tin-stripping wastewater I that contains more solid sediment, and this kind throw out is white, and main component is cassiterite (SnO
2), supernatant liquor is the green solution that contains a small amount of copper, but this tin-stripping wastewater storage is little.
The second is green muddy tin-stripping wastewater II.The characteristics of this kind tin-stripping wastewater II are obviously solid sediments of solution nothing itself, and solution is the colloidal sol shape than thickness, and proportion is 1.42～1.48g/cm
3, can see through common filter paper, only stay a small amount of sticky shape foreign material on the filter paper surface, this tin-stripping wastewater accounts for 85% left and right.Comparison of ingredients is complicated, mainly contains the metallic elements such as Sn, Cu, Fe, Pb, and its main component is 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 |
[0010]The third is the tin-stripping wastewater III after the long-term storage natural sedimentation, and a small amount of white cassiterite precipitation (SnO is arranged at its bottom
2), supernatant liquor is main cupric by analysis, and other component content is less, and its composition is as shown in table-2.
Analyzing the situation of above-mentioned three kinds of tin-stripping wastewaters can find out, tin-stripping wastewater I and tin-stripping wastewater III foreign matter content are few, and main component is comparatively single, relatively is easy to process.And tin-stripping wastewater II complicated component, several metals have certain content, and have higher reclamation value.Tin-stripping wastewater II is that in similar waste water, intractability is maximum but that output is the highest is a kind of.
Current, generally take ammonification or bicarbonate of ammonia neutralisation to process to tin-stripping wastewater, tin, iron, copper in tin-stripping wastewater are precipitated forms tin mud.This tin mud is sold relevant little smeltery as the raw material of reduction tin metallurgy and is processed.There is serious drawback in this treatment process, and the alkaline residue after precipitation is as the raw material of pyrometallurgical smelting on the one hand, and the valuable metal recovery utilization ratio is lower, and waste is serious, also has the risk of serious secondary pollution.
Also have maturing temperature higher (up to 850～950 ℃) in some techniques of processing tin-stripping wastewater, the reaction times is grown (2.5～5 hours), will certainly greatly increase energy consumption, not only increases cost, also is unfavorable for environment protection.
Therefore, for the character characteristics of circuit board tin-stripping wastewater, overcome the many disadvantages that existing processing mode exists, seek a kind of high efficiente callback and utilize its valuable metal and its innoxious method is had important practical significance.
Summary of the invention
In order to address the above problem, the invention provides a kind of method of utilizing tin-stripping wastewater to prepare sodium stannate, can overcome the defective of existing tin-stripping wastewater treatment process, simplify technique, significantly reduce energy consumption, reduced cost, can also obtain better quality product, obtain remarkable benefit.
This method of utilizing tin-stripping wastewater to prepare sodium stannate comprises the steps:
I, with the heavy mud oven dry of described tin-stripping wastewater solid-liquid separation gained, obtain raw material tin mud;
II, described tin mud and highly basic, water are mixed to mix 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 can dissolve described highly basic at least fully;
90～600 ℃ of III, control temperature, the described blank of roasting 2～4 hours forms siccative after cooling crush;
IV, be 1: 3～8 described siccative is mixed with water to form the first leach liquor according to mass ratio, control between 40～95 ℃ of temperature, then stirring reaction 1～6 hour carries out solid-liquid separation to described the first leach liquor and obtains the first filtrate and the first sediment;
V, to described the first filtrate evaporate, concentrate, crystallization; Obtain the sodium stannate crude product after cleaning described crystallization with strong base solution again;
VI, at 100～110 ℃ of temperature the described sodium stannate crude product of heating 2～3 hours, obtain the sodium stannate product.
Preferably, also comprise baking operation in described Step II I, concrete operations are that first to control temperature be to dry described blank in 60～130 ℃, 0.5～1.5 hour, and then progressively are increased to 90～600 ℃.
Preferably, the better practical range of described maturing temperature is 90～500 ℃.Low-temperature bake technique can significantly 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, be to be convenient to highly basic can evenly mix with tin mud adding of water, and the water consumption that can satisfy this purpose gets final product.Add entry too much unsuitable, otherwise can increase the temperature and time of subsequent step oven dry and roasting, 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 comprises that also secondary leaches operation: be 1: 2～12 described the first sediment to be mixed with water according to mass ratio, stirring reaction carries 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, to adding deslagging agent before described the first leach liquor solid-liquid separation, continue to stir 0.5～2 hour, described deslagging agent and the first leach liquor volume ratio are 1～20: 1000.Adding of deslagging agent is in order to remove the metal ions such as copper, iron.
Wherein, described deslagging agent raw material is generally water miscible sulfide, and commonly used is that mass concentration is 2～10% sodium sulphite or ammonium sulfide solution.
Wherein, also add the oxygenant of capacity in described the first filtrate, be used 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, and preparation condition is gentle, greatly reduces the maturing temperature of existing technique, has significantly reduced energy consumption, and effectively reduced cost effectively reduces the pollution to environment simultaneously; Technique is simply controlled, has simplified the leaching flow process, and has improved 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.
Description of drawings
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 is mainly the tin mud that precipitation from tin-stripping wastewater is formed, and mixes with alkaline solution at a certain temperature, through operations such as leaching, slagging-off, condensing crystal, protection oven dry, makes technical grade sodium stannate (Na
2SnO
33H
2O).
Embodiment 1
As shown in the figure, this method of 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 120 ℃ of left and right heating, dryings.This step can affect follow-up reaction mass, so must guarantee heavy mud finish-drying.Heavy mud after oven dry is the tin mud as reaction raw materials, is ground into powdery with pulverizer standby.Should heavy mud or tin argillization results of elemental analyses such 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 are mixed into blank with highly basic, water in mixing tank.
The present embodiment is got 100g tin mud, and water 50g is 1: 5 according to the ratio of tin atom and the amount of substance of hydroxide ion, and the add-on of calculating solid-state highly basic sodium hydroxide is about 68g.At first sodium hydroxide is dissolved in the water fully, then adds tin mud in this sodium hydroxide solution, stirring and evenly mixing forms the blank for the treatment of roasting.
III, oven dry and the described blank of roasting.
Above-mentioned blank is placed in stoving oven, drying program is set.At first control 100 ℃ of left and right the moisture in described blank is drained, process is about 1 hour; Then control temperature and be increased to 300 ℃, roasting 2～3 hours impels tin mud and highly basic fully to react.After roasting was completed, it is standby that cooling crush forms siccative.
IV, leaching Na
2SnO
3
Described siccative is transferred in batch extractor, is described siccative to be mixed with water in 1: 5 according to mass ratio, controls 60 ℃ of extraction temperatures, and stirring reaction 3 hours obtains the first leach liquor.At the leaching process coda, in order to remove the foreign ions such as cupric ion, iron ion, be added into appropriate deslagging agent in the first leach liquor, insulated and stirred 1 hour.The present embodiment deslagging agent is the sodium sulfide solution of mass concentration 5%, and addition is that every liter of first leach liquor adds the 10ml deslagging agent.
The first leach liquor after slagging-off is filtered, obtain the first filtrate and the first sediment.In gained the first filtrate, the leaching yield of tin can reach more than 90%, the results are shown in Table 2.
The content of tin in table 2 the first leach liquor, the first sediment, and tin leaching yield
In addition, owing to also containing more metal values element in the first sediment, as copper, iron etc., it is carried out the recyclable recycling of suitable processing.With suitable quantity of water, the first sediment is cleaned in the present embodiment, scavenging solution can be back to the dissolving that is used for solid-state highly basic in Step II.Then can carry out secondary to the first sediment and leach, be used for the recycling of metallic compound and alkali lye.
This secondary leaching process is: the mass ratio of adjusting the first sediment and water is 1:2～12; Stirring reaction 1～6 hour obtains the second leach liquor.To described the second leach liquor solid-liquid separation, after filtering, gained the 3rd filtrate can be back to the dissolving that is used 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, acquisition sodium stannate crude product.
The first filtrate is transferred to evaporating pot, adds appropriate oxygenant to make residual deslagging agent oxidation removal in the first filtrate.The oxygenant of the present embodiment is industrial hydrogen peroxide, can be with residual sulfide oxidation removal.Then heating makes described the first filtrate evaporation, treats that its concentrated solution is to two of stoste volume/for the moment, filtration obtains sodium stannate crystallisate and mother liquor thereof.The sodium stannate crystallisate cleans with 10～20% sodium hydroxide solution again, obtains the sodium stannate crude product.Mother liquor is recycled to the mixing jar.
Table 3 technical grade sodium stannate product detects 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 controls the described sodium stannate crude product of 100～110 ℃ of lower vacuum-dryings of temperature 2～3 hours, 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:
Can find out from upper data, the sodium stannate product that the present invention produces meets the technical grade product requirement.
For showing better technique of the present invention, the present invention also provides the embodiment of different sinter processs, and the sodium stannate product property that these embodiment obtain contrasts.Embodiment 2, embodiment 3, embodiment 4 and embodiment 5 are the oven dry of Step II I, the adjustment of sinter process parameter with the difference of embodiment 1.The various sodium stannate products of tin leaching yield detect analytical results 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 of different embodiment detects the analytical results contrast
By table 4, table 5 as can be known, at 90～500 ℃ of maturing temperatures, roasting time 2～3h, all can obtain the tin leaching yield more than 90%, and the sodium stannate quality product can be up to state standards all.And in actual applications, maturing temperature can also be increased to 600 ℃, namely is controlled in 90～600 ℃ of scopes all can reach better implementation result.
Embodiment 1 is only giving an example of more excellent processing step, it will be recognized by those skilled in the art that processing parameter can be adjusted to some extent in actual applications in a proper range, to adapt to the requirement of suitability for industrialized production.For example, the oven dry of tin mud is can be controlled in 100～130 ℃ of scopes, guarantee that moisture is thoroughly drained to get final product.Tin atom is controlled at 1: 4 with the ratio of the amount of substance of hydroxide ion～10 scopes in, the excessive leaching that can effectively promote tin of alkali lye, but also unnecessary consumption causes too greatly waste; Tin mud with add entry during highly basic mixes, be more even in order to allow highly basic mix, can guarantee therefore that highly basic dissolves fully to get final product, 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～and 8, extraction temperature can be controlled between 40～95 ℃.In addition, the deslagging agent that adds in leaching process can be selected 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, has significantly reduced energy consumption, and effectively reduced cost effectively reduces the pollution to environment simultaneously; Technique is simply controlled, has simplified the leaching flow process; And improved the leaching yield of tin, effectively optimized 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 (11)
1. a method of utilizing tin-stripping wastewater to prepare sodium stannate, comprise the steps:
I, with the heavy mud oven dry of described tin-stripping wastewater solid-liquid separation gained, obtain raw material tin mud;
II, described tin mud and highly basic, water are mixed to mix 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 can dissolve described highly basic at least fully;
90～600 ℃ of III, control temperature, the described blank of roasting 2～4 hours forms siccative after cooling crush;
IV, be 1: 3～8 described siccative is mixed with water to form the first leach liquor according to mass ratio, control between 40～95 ℃ of temperature, then stirring reaction 1～6 hour carries out solid-liquid separation to described the first leach liquor and obtains the first filtrate and the first sediment;
V, to described the first filtrate evaporate, concentrate, crystallization; Obtain the sodium stannate crude product after cleaning described crystallization with strong base solution again;
VI, at 100～110 ℃ of temperature the described sodium stannate crude product of heating 2～3 hours, obtain the sodium stannate product.
2. prepare according to claim 1 the method for sodium stannate, it is characterized in that, first control temperature before described Step II I and be 60～130 ℃, 0.5～1.5 hour and dry described blank, and then progressively be increased to 90～600 ℃.
3. the described method for preparing sodium stannate according to claim 1 and 2, is characterized in that, described maturing temperature is 90～500 ℃.
4. the described method for preparing sodium stannate according to claim 1 and 2, is characterized in that, described tin atom is 1: 5 with the ratio of the amount of substance of hydroxide ion.
5. the described method for preparing sodium stannate according to claim 1 and 2, is characterized in that, in described Step II, the mass ratio of tin mud and water is 1: 0.5～1.
6. the described method for preparing sodium stannate according to claim 1 and 2, is characterized in that, in described step IV, the mass ratio of siccative and water is 1: 5.
7. the described method for preparing sodium stannate according to claim 1 and 2, is characterized in that, described step IV comprises that also secondary leaches operation: be 1: 2～12 described the first sediment to be mixed with water according to mass ratio, stirring reaction carries out solid-liquid separation after 1～6 hour.
8. the described method for preparing sodium stannate according to claim 1 and 2, is characterized in that, to adding deslagging agent before described the first leach liquor solid-liquid separation, continues to stir 0.5～2 hour, and described deslagging agent and the first leach liquor volume ratio are 1～20: 1000.
9. prepare according to claim 8 the method for sodium stannate, it is characterized in that, described deslagging agent is that mass concentration is 2～10% sodium sulphite or ammonium sulfide solution.
10. prepare according to claim 9 the method for sodium stannate, it is characterized in that, also add the oxygenant of capacity in described the first filtrate, be used for removing excessive deslagging agent.
11. prepare according to claim 10 the method for sodium stannate, it is characterized in that, described oxygenant is hydrogen peroxide; Described highly basic is sodium hydroxide; The mass concentration of described step V strong base solution is 10～20%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232985A (en) * | 2022-07-01 | 2022-10-25 | 清远市中宇环保实业有限公司 | Novel alkaline leaching-crystallization preparation process for tin in tin-containing sludge |
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| FR2019653A1 (en) * | 1968-10-02 | 1970-07-03 | Goldschmidt Ag Th | |
| CN101497458A (en) * | 2008-01-30 | 2009-08-05 | 深圳市东江环保股份有限公司 | Method for preparing sodium stannate using circuit board tin-stripping wastewater |
| CN101532096A (en) * | 2009-04-01 | 2009-09-16 | 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 |
-
2013
- 2013-03-13 CN CN201310079993.1A patent/CN103172109B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2019653A1 (en) * | 1968-10-02 | 1970-07-03 | Goldschmidt Ag Th | |
| CN101497458A (en) * | 2008-01-30 | 2009-08-05 | 深圳市东江环保股份有限公司 | Method for preparing sodium stannate using circuit board tin-stripping wastewater |
| CN101532096A (en) * | 2009-04-01 | 2009-09-16 | 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 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232985A (en) * | 2022-07-01 | 2022-10-25 | 清远市中宇环保实业有限公司 | Novel alkaline leaching-crystallization preparation process for tin in tin-containing sludge |
| CN115232985B (en) * | 2022-07-01 | 2024-01-16 | 清远市中宇环保实业有限公司 | Alkaline leaching-crystallization preparation process of tin in tin-containing sludge |
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