CN102923752A - New method for decolorizing and whitening phosphogypsum - Google Patents
New method for decolorizing and whitening phosphogypsum Download PDFInfo
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- CN102923752A CN102923752A CN2012104614732A CN201210461473A CN102923752A CN 102923752 A CN102923752 A CN 102923752A CN 2012104614732 A CN2012104614732 A CN 2012104614732A CN 201210461473 A CN201210461473 A CN 201210461473A CN 102923752 A CN102923752 A CN 102923752A
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- phosphogypsum
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- decolorizing
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Abstract
The invention discloses method for decolorizing and whitening phosphogypsum. The method comprises the following steps: firstly, removing the organic impurities in the phosphogypsum through a calcination process under a suitable condition; secondly, carrying out decolorizing and whitening to the phosphogypsum by taking sulfuric acid and hydrochloric acid as pickling agents; and finally, carrying out filtering, washing and drying to obtain a whitened phosphogypsum sample. The method has the characteristics of simple operating process, low operating cost and good whitening effect, and opens a new way to the large-scale industrialized treatment and comprehensive utilization of discarded phosphogypsum.
Description
One, technical field
The present invention relates to the comprehensive utilization of industrial by-product phosphogypsum slag, exactly is the novel method that a kind of phosphogypsum decolouring is brightened.
Two, background technology
Phosphogypsum is the solid slag that produces in the Wet-process Phosphoric Acid Production process; every production 1t phosphoric acid need consume 2t sulfuric acid approximately; produce simultaneously 4 ~ 5t phosphogypsum; the annual discharging of China's sulphur dioxide of phosphor chemical industry phosphogypsum is about 5,000 ten thousand t; and just with annual 15% rate increase; the Eleventh Five-Year Plan period domestic enterprise's phosphogypsum comprehensive utilization ratio on average only is 20%; a considerable amount of phosphogypsums still take directly stacking form to dispose; a large amount of land resourcess have not only been taken; bring heavy burden to manufacturing enterprise; also caused larger environmental pollution, therefore from protection of the environment and technical security angle, the comprehensive utilization of phosphogypsum slag has more and more been paid close attention to.
The main component of phosphogypsum is CaSO
42H
2O, after suitably processing, not only can be used for preparing the plaster of Paris series product, such as gypsum sheet material (Thistle board, plaster board), gypsum block, building gypsum plaster, ceramic decoration material, gypsum building standard square and produce concrete retardation agent, cooperate with cement, sandstone as reinforcing weak subgrade material etc. such as gypsum, can also be used for making gypsum base electro-conductive material, gypsum base magneticsubstance, novel heat insulation material, the solid material of high-moisture quick-setting-mine weighting agent, New Phosphorus gypsum base polychloroethylene section bar etc.In addition, the phosphogypsum behind the purifying also can be used as various industrial fillers, such as papermaking filler, and siccative, the polishing material of casting mould and glass industry, the conditioning agent of gas concrete etc.
Phosphogypsum is because containing organic impurity, and a small amount of SiO
2With impurity metal ions such as iron, magnesium, aluminium, generally be pale yellow, light gray or grey black, whiteness is lower, has limited greatly it in industrial application.Along with the application of phosphogypsum in various industry, more and more higher to the requirement of gypsum whiteness during in particular for interior painting and decorated articles, the research that gypsum brightens also is subject to industry member and science researcher's attention gradually.
At present, the aspect that decolouring is brightened about phosphogypsum is rare bibliographical information still.
Three, summary of the invention
The present invention aims to provide the novel method that a kind of phosphogypsum decolouring is brightened, technical problem to be solved is to select suitable calcining process and acid leaching process to reach the purpose that decolouring is brightened, for new way is opened up in industrially scalable processing and the comprehensive utilization of using waste phosphorus gypsum.
Technical solution problem of the present invention adopts following technical scheme:
The novel method that phosphogypsum decolouring of the present invention is brightened comprises each unit process of calcining, acidleach and aftertreatment:
Described calcining is in 300-800 ℃ of calcining 30-150min with phosphogypsum;
Described acidleach is that the phosphogypsum after the calcining is placed pickling liquor, in 40-90 ℃ of acidleach 60-210min.
Described pickling liquor is the pickling agent solution of mass concentration 20-35%; Described pickling agent is selected from H
2SO
4, HCl, HNO
3, in the oxalic acid, acetic acid, citric acid one or more.
The mass ratio of pickling liquor and phosphogypsum is 2-4:1.
Described aftertreatment is that the mixed solution after acidleach is processed filters, washing, and filter cake dryly must brighten the phosphogypsum sample through 60 ℃.
The inventive method has the advantages that operating procedure is simple, running cost is low, whitening effect is good, for new way is opened up in industrially scalable processing and the comprehensive utilization of using waste phosphorus gypsum.
Four, embodiment
The phosphogypsum raw material that uses in the embodiment of the invention is the phosphogypsum powder that obtains after grinding through useless acid-treated solid using waste phosphorus gypsum in the phophatic fertilizer production process, and its chemical constitution is as shown in table 1:
The chemical constitution of table 1 phosphogypsum
| Composition | SiO 2 | P 2O 5 | CaO | MgO | T Fe | SO 3 | Other |
| Mass percent/% | 7.00 | 0.18 | 34.03 | 0.053 | 0.39 | 41.70 | 16.65 |
Embodiment 1:
The method that the phosphogypsum decolouring is brightened in the present embodiment is to operate as follows:
A, calcining
Phosphogypsum after taking by weighing 20g and grinding is placed in 550 ℃ the retort furnace in calcining crucible, high-temperature calcination 60min, and cooling, stand-by.
B, acidleach
Take by weighing phosphogypsum after the 10g step a gained calcining in the single port flask, add the sulphuric acid soln 40g of 30wt%, 90 ℃ of constant temperature, stirring reaction 180min, after reaction finishes, filtering separation, washing, dry, grind, must decolour and brighten phosphogypsum sample after the processing, surveying its whiteness is 87.1%.
Embodiment 2:
The method that the phosphogypsum decolouring is brightened in the present embodiment is to operate as follows:
A, calcining
Phosphogypsum after taking by weighing 20g and grinding is placed in 400 ℃ the retort furnace in calcining crucible, high-temperature calcination 40min, and cooling, stand-by.
B, acidleach
Take by weighing phosphogypsum after the 10g step a gained calcining in the single port flask, add the hydrochloric acid soln 40g of 35wt%, 85 ℃ of constant temperature, stirring reaction 150min, after reaction finishes, filtering separation, washing, dry, grind, must decolour and brighten phosphogypsum sample after the processing, surveying its whiteness is 79.8%.
Embodiment 3:
The method that the phosphogypsum decolouring is brightened in the present embodiment is to operate as follows:
A, calcining
Phosphogypsum after taking by weighing 20g and grinding is placed in 650 ℃ the retort furnace in calcining crucible, high-temperature calcination 70min, and cooling, stand-by.
B, acidleach
Take by weighing phosphogypsum after the 10g step a gained calcining in the single port flask, add the salpeter solution 40g of 25wt%, 90 ℃ of constant temperature, stirring reaction 120min, after reaction finishes, filtering separation, washing, dry, grind, must decolour and brighten phosphogypsum sample after the processing, surveying its whiteness is 81.9%.
Embodiment 4:
The method that the phosphogypsum decolouring is brightened in the present embodiment is to operate as follows:
A, calcining
Phosphogypsum after taking by weighing 20g and grinding is placed in 700 ℃ the retort furnace in calcining crucible, high-temperature calcination 50min, and cooling, stand-by.
B, acidleach
Take by weighing phosphogypsum after the 10g step a gained calcining in the single port flask, add the oxalic acid solution 40g of 20wt%, 85 ℃ of constant temperature, stirring reaction 210min, after reaction finishes, filtering separation, washing, dry, grind, must decolour and brighten phosphogypsum sample after the processing, surveying its whiteness is 80.6%.
Claims (3)
1. the novel method that the phosphogypsum decolouring is brightened comprises each unit process of calcining, acidleach and aftertreatment, it is characterized in that: described calcining is in 400-700 ℃ of calcining 35-85min with phosphogypsum;
Described acidleach is that the phosphogypsum after the calcining is placed pickling liquor, in 70-90 ℃ of acidleach 120-210min.
2. method according to claim 1 is characterized in that:
Described pickling liquor is the pickling agent solution of mass concentration 20-35%;
Described pickling agent is selected from H
2SO
4, HCl, HNO
3, in the oxalic acid, acetic acid, citric acid one or more.
3. method according to claim 1 and 2 is characterized in that:
The mass ratio of pickling liquor and phosphogypsum is 2-4:1.
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| CN2012104614732A CN102923752A (en) | 2012-11-15 | 2012-11-15 | New method for decolorizing and whitening phosphogypsum |
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| CN2012104614732A CN102923752A (en) | 2012-11-15 | 2012-11-15 | New method for decolorizing and whitening phosphogypsum |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524325A (en) * | 2014-09-28 | 2016-04-27 | 杨刚 | Novel utilization method of phosphogypsum |
| CN106348333A (en) * | 2016-08-31 | 2017-01-25 | 华中师范大学 | Method for recovering barium sulfate from desulfuration process for extracting and refining hosphoric acid by wet process |
| CN106854391A (en) * | 2017-01-17 | 2017-06-16 | 云南昆钢建设集团有限公司 | A kind of ardealite base inner wall putty powder and preparation method thereof |
| CN107674483A (en) * | 2017-10-17 | 2018-02-09 | 合肥工业大学 | A kind of Ardealite putty powder prepared by ardealite |
| CN109180036A (en) * | 2018-09-07 | 2019-01-11 | 昆明理工大学 | A kind of method that ardealite decoloration is brightened |
| CN110304852A (en) * | 2019-08-14 | 2019-10-08 | 江苏一夫科技股份有限公司 | A kind of method that desulfurized gypsum brightens and obtained gypsum and purposes |
| CN110528060A (en) * | 2019-08-28 | 2019-12-03 | 三明学院 | The method and calcium sulfate crystal whiskers of fluorgypsum slag growth calcium sulfate crystal whiskers |
| CN111792663A (en) * | 2020-07-15 | 2020-10-20 | 江苏一夫科技股份有限公司 | Ardealite whitening method |
| CN112279538A (en) * | 2020-11-02 | 2021-01-29 | 中南大学 | Method for extracting pollutants in gypsum slag by combined roasting-acid leaching |
| CN113213521A (en) * | 2021-05-12 | 2021-08-06 | 昆明理工大学 | Method for enhancing whiteness of waste gypsum |
| CN113620625A (en) * | 2021-09-15 | 2021-11-09 | 江苏一夫科技股份有限公司 | Method for removing impurities from phosphogypsum and preparing white anhydrous phosphogypsum |
| CN114477815A (en) * | 2022-03-03 | 2022-05-13 | 云南云天化股份有限公司 | Method for quickly whitening phosphogypsum |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105524325A (en) * | 2014-09-28 | 2016-04-27 | 杨刚 | Novel utilization method of phosphogypsum |
| CN105524325B (en) * | 2014-09-28 | 2018-03-30 | 杨刚 | A kind of Application way of ardealite |
| CN106348333A (en) * | 2016-08-31 | 2017-01-25 | 华中师范大学 | Method for recovering barium sulfate from desulfuration process for extracting and refining hosphoric acid by wet process |
| CN106348333B (en) * | 2016-08-31 | 2017-11-10 | 华中师范大学 | In extracting and refining phosphoric acid by wet process in desulfurization process barium sulfate recovery method |
| CN106854391A (en) * | 2017-01-17 | 2017-06-16 | 云南昆钢建设集团有限公司 | A kind of ardealite base inner wall putty powder and preparation method thereof |
| CN107674483A (en) * | 2017-10-17 | 2018-02-09 | 合肥工业大学 | A kind of Ardealite putty powder prepared by ardealite |
| CN109180036A (en) * | 2018-09-07 | 2019-01-11 | 昆明理工大学 | A kind of method that ardealite decoloration is brightened |
| CN110304852A (en) * | 2019-08-14 | 2019-10-08 | 江苏一夫科技股份有限公司 | A kind of method that desulfurized gypsum brightens and obtained gypsum and purposes |
| CN110528060A (en) * | 2019-08-28 | 2019-12-03 | 三明学院 | The method and calcium sulfate crystal whiskers of fluorgypsum slag growth calcium sulfate crystal whiskers |
| CN111792663A (en) * | 2020-07-15 | 2020-10-20 | 江苏一夫科技股份有限公司 | Ardealite whitening method |
| CN112279538A (en) * | 2020-11-02 | 2021-01-29 | 中南大学 | Method for extracting pollutants in gypsum slag by combined roasting-acid leaching |
| CN112279538B (en) * | 2020-11-02 | 2022-06-14 | 中南大学 | Method for extracting pollutants in gypsum slag by combined roasting-acid leaching |
| CN113213521A (en) * | 2021-05-12 | 2021-08-06 | 昆明理工大学 | Method for enhancing whiteness of waste gypsum |
| CN113620625A (en) * | 2021-09-15 | 2021-11-09 | 江苏一夫科技股份有限公司 | Method for removing impurities from phosphogypsum and preparing white anhydrous phosphogypsum |
| CN114477815A (en) * | 2022-03-03 | 2022-05-13 | 云南云天化股份有限公司 | Method for quickly whitening phosphogypsum |
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Application publication date: 20130213 |