CN102989402A - Method for reducing concentration of calcium ions in calcium-containing solution - Google Patents
Method for reducing concentration of calcium ions in calcium-containing solution Download PDFInfo
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- CN102989402A CN102989402A CN2011102689265A CN201110268926A CN102989402A CN 102989402 A CN102989402 A CN 102989402A CN 2011102689265 A CN2011102689265 A CN 2011102689265A CN 201110268926 A CN201110268926 A CN 201110268926A CN 102989402 A CN102989402 A CN 102989402A
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Abstract
The invention discloses a method for reducing the concentration of calcium ions in a calcium-containing solution. The method comprises the following steps: carrying out first contact of the calcium-containing solution and a calcium binder under a first contact condition, carrying out second contact of the product obtained after the first contact and a calcium separating agent under a second contact condition, and carrying out solid-liquid separation of the product obtained after the second contact, wherein the calcium binder is a substance which reacts with the calcium ions to form a precipitate, the calcium separating agent is a substance which enables the precipitate to aggregate, the first contact condition enables the content of the calcium ions in the product obtained after the first contact to be reduced to below 0.02g/L, and the second contact condition enables the content of calcium in the solution obtained after the second contact to be reduced to below 0.008g/L. The method has the advantages of convenient operation, simple technology, low equipment requirement, low cost, easy industrial application, low requirements of solution components, wide application range, good calcium removal effect and high product quality.
Description
Technical field
The present invention relates to the method that a kind of reduction contains calcium ion concentration in the calcium solution.
Background technology
Calcium is very wide in distributed in nature, and the industries such as metallurgy, chemical industry, medicine, the energy and environmental protection all relate to deliming technique, and are more and more higher to the requirement of calcium content in the ammonium metavanadate especially along with the development of denitrating catalyst, and is also more and more harsher to the requirement of deliming method.
Usually utilize the carbonate such as sodium carbonate to remove the calcium that contains in the calcium solution, the method is weak effect not only, but also has the sedimentation difficulty, easily wears the shortcomings such as filter.
Hou Xin just has been published in and has mentioned in " Jarosite Residues leachate reduction and deep purifying " literary composition on Lanzhou University of Science ﹠ Technology's journal and utilize the ammonium fluoride precipitation method to remove calcium in the Jarosite Residues leachate.Calcium content can be reduced to below the 0.005g/L after the method deliming, but fluorine ion is larger to the hazard ratio of the corrosion of equipment and environment, is unfavorable for using on the large industrial production.
In addition, said method does not all relate to the purification deliming method that vanadium titano-magnetite vanadium chromium solution, molten iron blow vanadium vanadium slag Leaching Vanadium liquid, extracting vanadium from stone coal vanadium liquid, thick vanadium product dissolving gained vanadium liquid and other calcic solution.
Summary of the invention
The object of the invention is to overcome the deficiency of existing deliming method, a kind of easy realization Separation of Solid and Liquid is provided, can cause corrosion and can be to the deliming method of environment to equipment.
The invention provides the method that a kind of reduction contains calcium ion concentration in the calcium solution, the method comprises that this is contained calcium solution carries out first with the calcium bond and contact, and the first contact products therefrom carried out second with the calcium release agent and contact, and with second the contact products therefrom carry out Separation of Solid and Liquid, described calcium bond is the material that can form with the calcium ion reaction precipitation, described calcium release agent is the material that described precipitation is assembled, the condition of described the first contact so that the calcium ion content of the first contact in the products therefrom be reduced to below the 0.02g/L, the condition of described the second contact so that the calcium content in the second contact gained solution be reduced to below the 0.008g/L.
Method of the present invention compared with prior art has following beneficial effect: not can to equipment cause the corrosion and can be to environment; Solution composition requires loose, wide accommodation, be applicable to the purification deliming that vanadium titano-magnetite vanadium chromium solution, molten iron blow vanadium vanadium slag Leaching Vanadium liquid, extracting vanadium from stone coal vanadium liquid, thick vanadium product dissolving gained vanadium liquid and other calcic solution, realize the removal of calcium in the calcium vanadium solution, filled up the vacancy of deliming technology in the present calcium vanadium solution; Deliming is effective, and product quality is high; The separating step of sediment and solution is simple among the present invention, and is easy to operate, and equipment requirement is low; Technique is simple, and cost is low, is easy to apply industrial.
Other features and advantages of the present invention will partly be described in detail in the specific embodiment subsequently.
The specific embodiment
The invention provides the method that a kind of reduction contains calcium ion concentration in the calcium solution, the method comprises that this is contained calcium solution carries out first with the calcium bond and contact, and the first contact products therefrom carried out second with the calcium release agent and contact, and with second the contact products therefrom carry out Separation of Solid and Liquid, described calcium bond is the material that can form with the calcium ion reaction precipitation, described calcium release agent is the material that described precipitation is assembled, the condition of described the first contact is so that the calcium ion content of the first contact in the products therefrom is reduced to 0.02g/L, the condition of described the second contact so that the calcium content in the second contact gained solution be reduced to below the 0.008g/L.
Among the present invention, calcium ion content refers in the solution content of the calcium that exists with free calcium ion form, generally adopts atomic absorption spectrophotometry to record.Calcium content then refers to the total content of calcium constituent in the solution, comprises the calcium of free ionic species and the amount of the calcium that exists with precipitation form, generally adopts permanganimetric method to record.Equate with calcium content for the general calcium ion content of calcium solution that contains before processing, contact products therefrom and the second product of contact for first, calcium ion content is generally less than or equals calcium content.
According to the present invention, as long as make the described calcium solution that contains contact with the calcium release agent with the calcium bond successively and can realize purpose of the present invention, the consumption of described calcium bond can be selected in relative broad range, under the preferable case, the weight ratio of the calcium ion in the described solution and calcium bond is 1: (5-50), and more preferably 1: (5-15).
According to the present invention, as long as described calcium bond can form precipitation with the calcium ion reaction, under the preferable case, described calcium bond is one or more in oxalic acid and the water-soluble oxalates, more preferably one or more in oxalic acid, sodium oxalate, potassium oxalate and the ammonium oxalate.Compare with using other calcium bonds, use the calcium content in the solution after above-mentioned calcium bond can further reduce processing.
According to the present invention, the purpose of described the first contact is to make described calcium ion and the calcium bond that contains in the calcium solution to form precipitation, therefore the condition of described the first contact can be selected in relative broad range, as long as can achieve the above object, wherein, described the first contact more abundant (being that the time is longer), the deliming effect is better; Temperature is higher, and the deliming effect is also better.But under the preferable case, the condition of described the first contact comprise temperature be 60 ℃ to the boiling temperature of solution, the pH value is 3-11,5-10 more preferably, the time is 20-100 minute, is preferably 20-60 minute.
According to method provided by the invention, as long as make the described calcium solution that contains contact with the calcium release agent with the calcium bond successively and can realize purpose of the present invention, the consumption of described calcium release agent can be selected in relative broad range, under the preferable case, the weight ratio of the calcium ion in the described solution and calcium release agent is 1: (1-10), and more preferably 1: (1-5).
According to method provided by the invention, as long as described calcium release agent can promote sediment to assemble, for example, can be active carbon, polyacrylamide, gather in metasilicate Flocculant:, polyacrylic acid, Sodium Polyacrylate, the ligninsulfonate one or more.Under the preferable case, described calcium release agent is the combination of active carbon and polyacrylamide, and further the weight ratio of optimization polypropylene acid amides and active carbon is 1: (10-50).Use above-mentioned calcium release agent can obviously promote sedimentation, and follow-up filtration is carried out easily, when shortening filtration time, can also effectively prevent from wearing filter and filter incomplete phenomenon.
According to the present invention, described active carbon can also can be post grain active carbon for granular activated carbon, and the specific area of preferred described active carbon is 1000-2000m
2/ g, granularity is 12-50 μ m.Use above-mentioned preferred active carbon can further shorten deliming reaction time and prevent from wearing filter, filter easily row of safety thereby make.
According to the present invention, described polyacrylamide can be various types of polyacrylamides, is non-ionic polyacrylamide under the preferable case.The present inventor finds, uses the polyacrylamide of higher molecular weight further to shorten flocculation time, make deliming more thorough, so the weight average molecular weight of the preferred non-ionic polyacrylamide of the present invention is greater than 3,000,000.During use, can directly add Polyacrylamide Powder also can be with the polyacrylamide wiring solution-forming, under the preferable case, be mixed with solution and use, and concentration is 1-20g/L, is preferably 5-10g/L.
According to the present invention, reunite fast under the effect that the purpose of described the second contact is to make described the first contact gained be deposited in the calcium release agent, form bulky grain, therefore the condition of described the second contact can be selected in relative broad range, as long as can achieve the above object, under the preferable case, the condition of described the second contact comprises that temperature can be environment temperature, the pH nature is preferably 5-10.In order to obtain better balance between efficient and deliming rate, the time of preferred described the second contact is 20-60 minute.
According to the present invention, described contain calcium solution can for any calcium ion concentration in the 0.1-1.5g/L scope, the concentration of vanadium ion is calcic and the vanadium solution of 5-50g/L, is preferably vanadium titano-magnetite vanadium chromium solution, molten iron and blows in vanadium vanadium slag Leaching Vanadium liquid, extracting vanadium from stone coal vanadium liquid, the thick vanadium product dissolving gained vanadium liquid one or more.
The present invention is further illustrated below in conjunction with embodiment.
The used calcium solution that contains of embodiment 1-7 is common vanadium solution A, the embodiment 8 used calcium solutions that contain are that molten iron blows vanadium vanadium slag Leaching Vanadium liquid B, the embodiment 9 used calcium solutions that contain are extracting vanadium from stone coal vanadium liquid C, the embodiment 10 used calcium solutions that contain are thick vanadium dissolving gained vanadium liquid D, their main chemical compositions is as shown in table 1, and unit is gL
-1Embodiment 10 used solution are that concentration is the CaCl of 1.5g/L
2The aqueous solution.In following examples, polyacrylamide is available from Shanghai constant force material for water treatment Co., Ltd, and active carbon is available from the auspicious special material for water treatment in Gongyi City Co., Ltd.
Table 1
| V 5+ | P | Mg 2+ | Na + | Si | TFe | TCr | Mn | Al 3+ | Ca 2+ | pH | |
| A | 33.86 | 0.052 | 0.002 | 28.04 | 1.19 | 0.010 | 1.51 | 0.001 | 0.002 | 0.122 | 10.45 |
| B | 33.56 | 0.043 | 0.002 | 29.45 | 1.26 | 0.010 | 1.56 | 0.001 | 0.001 | 0.140 | 10.89 |
| C | 43.4 | 0.04 | 0.01 | 10.10 | 0.06 | 0.005 | 0.01 | 0.01 | 0.05 | 1.12 | 13.65 |
| D | 48.10 | 0.01 | 0.002 | 37.85 | 0.072 | 0.010 | 0.05 | 0.01 | 0.01 | 0.22 | 11.20 |
Embodiment 1
Add the common vanadium solution A in the 1000ml table 1 in the clean beaker of 2000ml, working concentration be the watery hydrochloric acid of 10% (quality) to regulate its pH be 5, be heated to 60 ℃, stir, add the 1.89g ammonium oxalate, behind the reaction 20min, pH is 5.2, and calcium ion content is 0.02g/L.Then add the polyacrylamide that 2ml concentration is 5g/L (weight average molecular weight greater than 3,000,000, nonionic) solution and 0.13g active carbon (specific area 1000m
2/ g, granularity are less than 50 μ m), reaction 20min, sedimentation is filtered, and obtaining calcium content is the low calcium vanadium solution of 0.005g/L.
Embodiment 2
Add the common vanadium solution A in the 1000ml table 1 in the clean beaker of 2000ml, working concentration be the watery hydrochloric acid of 10% (quality) to regulate its pH be 10, be heated to 60 ℃, stir, add the 6.1g sodium oxalate, behind the reaction 100min, pH is 10.22, and calcium ion content is 0.01g/L.Add the polyacrylamide that 4ml concentration is 10g/L (weight average molecular weight greater than 8,000,000, nonionic) solution and 1.2g active carbon (specific area 2000m
2/ g, granularity are less than 40 μ m), reaction 60min, sedimentation is filtered, and obtains the low calcium vanadium solution of calcium content 0.004g/L.
Embodiment 3
Add the common vanadium solution A in the 1000ml table 1 in the clean beaker of 2000ml, working concentration be the watery hydrochloric acid of 10% (quality) to regulate its pH be 9, be heated to 90 ℃, stir, add the 5.06g potassium oxalate, behind the reaction 30min, pH is 9.25, and calcium ion content is 0.01g/L.Add the polyacrylamide that 2ml concentration is 8g/L (weight average molecular weight greater than 3,000,000, nonionic) solution and 0.24g active carbon (specific area 1500m
2/ g, granularity are less than 50 μ m), reaction 60min, sedimentation is filtered, and obtains the low calcium vanadium solution of calcium content 0.005g/L.
Comparative Examples 1
Method according to embodiment 3 is carried out deliming to common vanadium solution A, and different is, does not add polyacrylamide and active carbon as the calcium release agent, and directly is that the first product of contact of 0.01g/L is carried out sedimentation and filtered with calcium ion content.As a result, the rate of filtration is very slow, and calcium content is 0.08g/L in the filtrate.
Embodiment 4
Method according to embodiment 3 is carried out deliming to common vanadium solution A, and different is that the 5.06g potassium oxalate is replaced by the 5.06g potassium phosphate, obtains the calcium vanadium solution of calcium content 0.006g/L.
Embodiment 5
Method according to embodiment 3 is carried out deliming to common vanadium solution A, and different is, 2ml concentration is that the polyacrylamide solution of 8g/L and 0.24g active carbon are by 0.5g active carbon (specific area 500m
2/ g, granularity are less than 50 μ m) replace, obtain the calcium vanadium solution of calcium content 0.008g/L.
Embodiment 6
Method according to embodiment 3 is carried out deliming to common vanadium solution A, different is, 2ml concentration is the polyacrylamide solution of 8g/L and 0.24g active carbon by 2ml concentration is that polyacrylamide (weight average molecular weight greater than 8,000,000, the nonionic) solution of 1g/L replaces, and obtains the calcium vanadium solution of calcium content 0.007g/L.
Embodiment 7
Method according to embodiment 3 is carried out deliming to common vanadium solution A, and different is, uses 5g polyaluminium sulfate (weight average molecular weight greater than 8,000,000, Beijing polyaluminum sulfate aluminium manufacturer) as the calcium release agent, to obtain the calcium vanadium solution of calcium content calcium content 0.008g/L.
Embodiment 8
Add 1000ml calcic solution B in the clean beaker of 2000ml, regulating its pH is 9, is heated to 80 ℃, stirs, and adds the 5g sodium oxalate, and behind the reaction 30min, pH is 9.25, and calcium ion content is 0.01g/L.Add the polyacrylamide that 2ml concentration is 6g/L (weight average molecular weight greater than 4,000,000, nonionic) solution and 0.5g active carbon (specific area 1500m
2/ g, granularity are less than 50 μ m), reaction 40min, sedimentation is filtered, and obtains the low calcium solution of calcium content 0.005g/L.
Embodiment 9
Add 1000ml calcic solution C in the clean beaker of 2000ml, regulating its pH is 9, is heated to boiling, stirs, and adds the 17.36g ammonium oxalate, and behind the reaction 60min, pH is 8.92, and calcium ion content is 0.02g/L.Add the polyacrylamide that 10ml concentration is 10g/L (weight average molecular weight greater than 3,000,000, nonionic) solution and 5g active carbon (specific area 1500m
2/ g, granularity are less than 50 μ m), reaction 60min, sedimentation is filtered, and obtains the low calcium solution of calcium content 0.005g/L.
Embodiment 10
Add 1000ml calcic solution D in the clean beaker of 2000ml, regulating its pH is 9, is heated to 80 ℃, stirs, and adds the 6g sodium oxalate, and behind the reaction 30min, pH is 9.25, and calcium ion content is 0.01g/L.Add the polyacrylamide that 15ml concentration is 8g/L (weight average molecular weight greater than 3,000,000, nonionic) solution and 1.2g active carbon (specific area 1000m
2/ g, granularity are less than 50 μ m), reaction 60min, sedimentation is filtered, and obtains the low calcium solution of calcium content 0.005g/L.
Embodiment 11
Adding 1000ml concentration in the clean beaker of 2000ml is the CaCl of 1.5g/L
2The aqueous solution, regulating its pH is 9, is heated to 70 ℃, stirs, and adds the 7.5g potassium oxalate, behind the reaction 60min, pH is that 9.55 calcium ion contents are 0.02g/L.Add the polyacrylamide that 5ml concentration is 10g/L (average molecular weight greater than 8,000,000, nonionic) solution and 2.5g active carbon (specific area 1500m
2/ g, granularity are less than 50 μ m), reaction 60min, sedimentation is filtered, and obtains the low calcium solution of calcium content 0.005g/L.
From above-described embodiment, can find out, method of the present invention not only can reduce the content that contains calcium in the calcium solution, but also have free settling, not etching apparatus and advantage free from environmental pollution, and with the preferred calcium bond of non-the present invention and calcium release agent, the deliming effect does not all reach below the calcium content 0.005g/L.
Below describe in conjunction with the embodiments preferred embodiment of the present invention in detail; but; the present invention is not limited to the detail in the above-mentioned embodiment; in technical conceive scope of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Need to prove in addition, each concrete technical characterictic described in the above-mentioned specific embodiment in reconcilable situation, can make up by any suitable mode, for fear of unnecessary repetition, the present invention is to the no longer separately explanation of various possible combinations.
It in addition, also can carry out any combination between the various embodiment of the present invention, as long as without prejudice to thought of the present invention, should be considered as content disclosed in this invention equally.
Claims (12)
1. a reduction contains the method for calcium ion concentration in the calcium solution, the method comprises that this is contained calcium solution carries out first with the calcium bond and contact, and the first contact products therefrom carried out second with the calcium release agent and contact, and with second the contact products therefrom carry out Separation of Solid and Liquid, described calcium bond is the material that can form with the calcium ion reaction precipitation, described calcium release agent is the material that described precipitation is assembled, the condition of described the first contact so that in the first contact products therefrom calcium ion content be reduced to below the 0.02g/L, the condition of described the second contact so that in the second contact gained solution calcium content be reduced to below the 0.008g/L.
2. method according to claim 1 wherein, describedly contains calcium ion in the calcium solution and the weight ratio of calcium bond is 1: 5-50.
3. method according to claim 1 and 2, wherein, described calcium bond is one or more in oxalic acid and the water-soluble oxalates.
4. method according to claim 3, wherein, described calcium bond is one or more in oxalic acid, sodium oxalate, potassium oxalate and the ammonium oxalate.
5. the described method of any one according to claim 1-4, wherein, described first the contact condition comprise temperature be 60 ℃ to the boiling temperature that contains calcium solution, the pH value is 5-10, the time is 20-100 minute.
6. the described method of any one according to claim 1-5 wherein, describedly contains calcium ion in the calcium solution and the weight ratio of calcium release agent is 1: 1-10.
7. the described method of any one according to claim 1-6, wherein, described calcium release agent is active carbon and polyacrylamide, and the weight ratio of polyacrylamide and active carbon is 1: 10-50.
8. method according to claim 7, wherein, the specific area of described active carbon is 1000-2000m
2/ g, granularity is 12-50 μ m.
9. method according to claim 7, wherein, described polyacrylamide is non-ionic polyacrylamide, and the weight average molecular weight of this non-ionic polyacrylamide is greater than 3,000,000.
10. the described method of any one according to claim 7-9, wherein, the condition of described the second contact comprises that the time is 20-60 minute.
11. the described method of any one according to claim 1-9, wherein, the described calcium solution that contains is the solution that contains vanadium and calcium, and wherein the concentration of calcium ion is 0.1-1.5g/L, and the concentration of vanadium ion is 5-50g/L.
12. the described method of any one according to claim 1-11, wherein, the described calcium solution that contains is that vanadium titano-magnetite vanadium chromium solution, molten iron blow one or more in vanadium vanadium slag Leaching Vanadium liquid, extracting vanadium from stone coal vanadium liquid, the thick vanadium product dissolving gained vanadium liquid.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103409627A (en) * | 2013-07-09 | 2013-11-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing low-silicon low-calcium low-aluminium vanadium liquid |
| CN112195347A (en) * | 2020-09-27 | 2021-01-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
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| CN1066830A (en) * | 1992-06-23 | 1992-12-09 | 中国核工业总公司北京核仪器厂 | purification method of high-purity sodium iodide |
| CN101428929A (en) * | 2008-12-09 | 2009-05-13 | 中南大学 | Method for direct advanced treatment for heavy metal wastewater with biological agent |
| CN101555053A (en) * | 2008-04-11 | 2009-10-14 | 中国科学院广州地球化学研究所 | Compound coagulant used for treating rare-earth highly concentrated ammonian wastewater to recover industry ammonium chloride and treatment method |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0129259A1 (en) * | 1983-04-29 | 1984-12-27 | Laboratorium Für Adsorptionstechnik Gmbh | Activated carbon product |
| CN1066830A (en) * | 1992-06-23 | 1992-12-09 | 中国核工业总公司北京核仪器厂 | purification method of high-purity sodium iodide |
| CN101555053A (en) * | 2008-04-11 | 2009-10-14 | 中国科学院广州地球化学研究所 | Compound coagulant used for treating rare-earth highly concentrated ammonian wastewater to recover industry ammonium chloride and treatment method |
| CN101428929A (en) * | 2008-12-09 | 2009-05-13 | 中南大学 | Method for direct advanced treatment for heavy metal wastewater with biological agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103409627A (en) * | 2013-07-09 | 2013-11-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing low-silicon low-calcium low-aluminium vanadium liquid |
| CN112195347A (en) * | 2020-09-27 | 2021-01-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium extraction method of calcified vanadium slag |
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