CN1765837A - Potash feldspar wet method decomposition and production process - Google Patents
Potash feldspar wet method decomposition and production process Download PDFInfo
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Abstract
The wet-way decomposition manufacturing technique for potash feldspar comprises: adding sulfuric acid into the mineral powder of potash feldspar and fluorite to mix and acidolysis at 50-80Deg, preparing white carbon black both from gas and acidolysis liquid to increase its yield as well as aluminum hydroxide and sodium fluoride and K-N compound fertilizer. This process is simple, high effect and low cost, can produce a plurality of products and byproducts with little pollution well economic benefit.
Description
Technical Field
The invention relates to a potash fertilizer production technology, also relates to a production process of inorganic chemical raw materials, and particularly relates to a wet decomposition production process of potash feldspar.
Technical Field
The potash feldspar is a natural ore rich in potassium, aluminum and silicon elements,the potash feldspar ore is abundant in China, and many enterprises use the potash feldspar as an additive for producing cement, ceramic or glass, so that the added value is low. In recent ten years, China has made some progress in the aspect of comprehensive development and utilization of potassium feldspar, wherein the wet decomposition process of potassium feldspar can simultaneously produce by-products of chemical raw materials such as white carbon black, polyaluminium chloride and the like in the process of preparing potassium sulfate. For example, Chinese patent publication No.: CN1072197C, announcement date: day 3, 110 month 2001, invention name: a wet decomposing method for potash feldspar ore includes such steps as reaction between potash feldspar and inorganic acid and fluoride under stirring at ordinary pressure and low temp, separation, calcining the solid phase containing potassium sulfate, aluminium oxide and silicon dioxide, and further processing to obtain ammonia, aluminium and silicon potassium sulfate series products.
Chinese patent publication No.: CN 1557781a, published: 12 and 29 in 2004, invention name: a low-temperature decomposition method for potassium feldspar proposes that potassium feldspar, sulfuric acid and an auxiliary agent fluosilicic acid are mixed and react at the temperature of 90-150 ℃ to generate silicon tetrafluoride gas and soluble salts, and the silicon tetrafluoride gas is absorbed by a four-stage system to obtain silicic acid precipitate which can be processed into white carbon black; the soluble salts are neutralized to generate potassium ion solution and aluminum hydroxide precipitate, and the potassium ammonium sulfate compound fertilizer and the polymeric aluminum sulfate can be prepared respectively. The method has the advantages of improving the comprehensive utilization rate of the potassium feldspar, along with simple process and high recovery utilization rate of the auxiliary agent, but the method has the disadvantages of complicated recovery of silicon-containing gas, less amount of recovered silicic acid and prepared white carbon black, insufficient utilization of silicon compounds contained in the potassium feldspar, higher cost of the auxiliary agent, incomplete decomposition of ores, and low yield and quality of prepared products and byproducts.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a wet decomposition production process for potassium feldspar. The method has simple process, and the produced white carbon black product has high yield and good quality; the produced aluminum hydroxide, potassium-nitrogen compound fertilizer and other byproducts have more varieties, good quality, less emission in the whole process and less environmental pollution.
The technical solution of the invention is as follows: the potassium feldspar wet decomposition production process comprises the following steps:
1) adding feldspar powder into fluorite powder and a small amount of water, mixing and stirring into paste, gradually adding sulfuric acid, and stirring at 50-80 ℃ for acidolysis reaction to generate silicon-containing gas and solid-phase residue;
2) inputting the silicon-containing gas generated in the step 1) into a Venturi absorber for absorption, adding ammonia water into absorption liquid for neutralization, and washing, drying and crushing the filtered precipitate to obtain fumed silica;
3) filtering and separating the acidolysis solution and the solid-phase residue in the step 1), and washing the solid-phase residue to obtain gypsum;
4) adding ammonia water into the filtered and washed liquid in the step 3) for neutralization, adjusting the pH value to 9-9.5, curing at the temperature of 70-80 ℃, and filtering to obtain a precipitate;
5) adding sulfuric acid into the precipitate obtained in the step 4), reacting, washing with water, filtering, drying and crushing to obtain the liquid-phase white carbon black;
6) adding ammonia water into the filtering and washing liquid obtained in the step 5) for neutralization, curing at the temperature of 70-80 ℃, filtering, washing, drying the filtered precipitate, and crushing to obtain aluminum hydroxide;
7) evaporating the filtrate and the washing liquid in the step 5) or the step 6), cooling, crystallizing and filtering to obtain the K-N compound fertilizer.
In the step 1) of the invention, the potash feldspar ore powder, fluorite powder and sulfuric acid are added according to the proportion (weight parts) of 1: 1-2: 2-3.
In the invention, in the step 1), the absorption liquid filtered out in the step 2) is added firstly, and then sulfuric acid is added.
The curing time in the step 4) and the step 6) of the invention is 30-60 minutes.
The drying in the step 2), the step 5) and the step 6) is vacuum low-temperature drying, and the drying temperature is 65-80 ℃.
Evaporating the filtered liquid in the step 4), adding sodium carbonate for synthesis, cooling for crystallization, and filtering to obtain the sodium fluoride.
In the invention, the filtration in the step 2), the step 5) and the step 6) adopts filter pressing.
In the invention, warm water with the temperature of 40-80 ℃ is adopted for washing in the step 2), the step 5) and the step 6).
The invention has the advantages that; 1, the white carbon black is prepared by gas, and meanwhile, the acidolysis reaction is carried out in a liquid phase, and the gas containing silicon is easily dissolved in water to form a silicon compound, so that the process route for preparing the white carbon black by acidolysis liquid is increased, the yield of the white carbon black is improved, the quality of an aluminum hydroxide product is also improved, a sodium fluoride product can be produced as a byproduct, and the comprehensive utilization rate of the potassium feldspar is high; and 2, the white carbon black (silicon dioxide) is absorbed from the gas by adopting a Venturi absorber and ammonia water neutralization mode, the process is simple and convenient, the control is easy, the absorption effect is good, and the neutralized liquid can be reused in the ore acidolysis reaction process so as to reduce the addition amount of a mineral additive, namely fluorite. 3, the prepared white carbon black, aluminum hydroxide and other products have higher purity, the total potassium content in the prepared potassium-nitrogen compound fertilizer is close to a theoretical value, and the potassium content and the nitrogen content are both higher. 4, the main emissions of the whole set of production process are liquid waste water containing potassium and ammonia, the evaporation for preparing the potassium-nitrogen compound fertilizer due to low concentration is economically unpractical, and if the potassium-nitrogen compound fertilizer is directly discharged, the potassium-nitrogen compound fertilizer has pollution to the environment, but can be applied to farmlands as the liquid potassium-nitrogen fertilizer, and has less pollution to the environment. 5, the whole set of production process is reasonable in arrangement, simple in flow, less in equipment investment, more in variety of main products and by-products, higher in yield and quality and considerable in economic benefit.
Drawings
FIG.1 is a flow chart of the production process of the present invention
Detailed Description
The invention is described in further detail below with reference to the following figures and detailed description:
1. pretreatment of ores
The potassium feldspar has a very compact lattice structure and very stable chemical properties. In the implementation process, locally produced carnosic potash feldspar ore is selected as a main raw material, and K in the ore2The average content of O is more than 10.5 percent and SiO2Average content of 66% Al2O3Average content of 15% Fe2O3The average content is in the range of 3% -4%. Potassium feldsparThe ore should be kept dry and not placed in the open air to prevent moisture from entering and affecting the pulverization, and the ore is coarsely pulverized and ball-milled to 200 meshes (full sieving). Mineral powder passing through 200 meshes can be selected as a raw material to increase the contact area with substances such as acid and the like. Because the ore contains Fe2O3Since impurities such as FeO have a dark color, iron removal and concentration treatment are required before the acidolysis reaction. The iron removal of the potassium feldspar can adopt different methods. The iron removing process includes stirring mineral powder, industrial sulfuric acid or hydrochloric acid and water at 50-80 deg.c to react, dissolving the impurity, such as iron, in the mineral powder in the sulfuric acid or hydrochloric acid, reaction, filtering and washing the mineral powder. Tests show that the smaller fineness of the mineral powder can also promote the reaction speed between iron removal and acidolysis. In the specific operation, putting the mineral powder intoan iron removal reaction tank, adding a proper amount of water and hydrochloric acid, maintaining the reaction temperature at 60-65 ℃, carrying out iron removal reaction, filtering after 2 hours, and washing until no floating matters exist. The mother liquor and the washing liquid can be used for preparing iron series products such as iron oxide red and the like. The process method for deironing and concentrating the potassium feldspar and producing the iron oxide red belongs to the invention creation completed by the self research of the applicant, and the invention creation is applied for patent by the applicant to the patent office of the national intellectual property office on the same day. The method has the advantages of good concentration effect, high utilization rate of the active ingredients of the potash feldspar ore, high iron recovery rate and little environmental pollution. Fe in potassium feldspar ore2O3The content of the acid-soluble organic acid is low, and the acid-soluble organic acid-soluble.
2. Acidolysis reaction of ore
Referring to fig. 1, the iron-removed and selected mineral powder, fluorite and sulfuric acid are prepared according to the proportion of 1: 1.8: 3 (the adding amount of fluorite and sulfuric acid is reduced in the subsequent acidolysis reaction), the mineral powder and fluorite powder are added with a small amount of water to be stirred and mixed into paste, then the sulfuric acid is gradually added, the reactant reaches the initial reaction temperature of 60-65 ℃ by means of the dilution heat of the sulfuric acid, and the acidolysis reaction temperature is maintained within the range of 65-70 ℃ or a little higher. During the reaction, water in proper amount may be added to maintain the solubility of the reactant, and steam may be introduced to heat the reactant to maintain the reaction temperature. During the acidolysis reaction, the materials react with each other more violently:
escaped SiX4Venturi absorber for gas and NH4And (3) absorbing the solution X:
(NH4)2SiX6the solution and ammonia water are subjected to neutralization reaction, and SiO is precipitated2.nH2O：
When the slurry of reactants turns white, the reaction is nearly complete. The precipitated silica is filtered, dried and crushed to prepare the fumed silica product. Filtering to separate SiO2.nH2The mother liquor after O contains a large amount of NH4X, if more absorption liquid is generated during the absorption and neutralization process, a part of the X can be used for absorbing SiX4The other part of the gas is used for participating in the reaction of acidolysis ore powder. Thus, more sulfuric acid and fluorite can be saved, and the production cost is greatly reduced.
The acidolysis washing liquid after the acidolysis reaction is filtered and washed by adding water enters the subsequent liquid-phase white carbon black production process for further decomposition and extraction, and the filtered solid matter and the solid-phase residue of the acidolysis reaction are gypsum which is a byproduct. In order to reduce potassium residue in gypsum, hot water of 60-80 deg.C is used to wash solid phase residue for the first time to reduce K2O is more soluble in the washing solution and can be washed with cold water for the second time.
Since the acidolysis reaction is carried out in a liquid phase environment, the escaping gas SiX is inevitably generated4Dissolved in water to form H2SiX6Filtering to remove CaSO4The mother liquor after (gypsum) is prepared from H2SiX6，K2SO4，Al2(SO4)3And the like, and the extraction is carried out in steps during subsequent treatment.
3. Neutralization process of acidolysis solution
As mentioned above, the gas discharged from the upper part of the acidolysis reaction tank is SiX4Available in the subsequent process containing NH4The mother liquid of X is absorbed by a Venturi absorber to generate (NH)4)2SiX6(NH4PH of X solution 5.5, 8-9%). Will be (NH)4)2SiX6Neutralizing with ammonia water to precipitate SiO2.nH2O and form NH4X mother liquor, and the processes are easy to carry out and control. As long as the operation is proper, a better operation effect can be achieved.
In the acidolysis process, silicon is absorbed in two different ways in the gas phase and the liquid phase, respectively, and the treatment of the gas phase silicon compound has been described above, and only the treatment of the silicon compound dissolved in the liquid phase with aluminum sulfate is described here:
adding ammonia water into the filtered acidolysis solution and the washing solution for neutralization reaction, wherein the reaction formula is as follows:
the neutralization is carried out in such a way that the pH of the solution is 9-9.5, i.e. the Al in the liquid phase is neutralized2(SO4)3Precipitating with silicon compound to reduce loss, and evaporating the filtered mother liquid to crystallize the potassium-nitrogen compound fertilizer. Due to Al (OH)3Dissolved in H2SO4So that the filtered precipitate is washed with 15-20% dilute sulfuric acid solution to dissolve Al (OH) in the precipitate3Then washing with soft water until the precipitate is free of SO4 2-Drying and crushing to obtain the white carbon black product. It should be noted that the precipitate generated in the neutralization process should be completely reacted by aging (70-80 deg.C) the neutralized ammonia solution for 30 min to prevent the precipitate from wrapping.
Mixing the dilute sulfuric acid filtrate and the washing liquid, adding ammonia water to neutralizepH 9-9.5, this time Al (OH) precipitated separately3Aging, filtering, and washing until no SO is generated4 2-Drying and crushing to obtain the aluminum hydroxide product. In the process of preparing the white carbon black product and the aluminum hydroxide product, the filtration can adopt a filter pressing mode; the washing can be carried out by warm water (40-60 ℃), and generally 3-5 times. The washing liquid can be checked by using a 5% barium chloride solution, if no white precipitate exists, the washing is qualified, otherwise, the washing is required to be carried out again; the drying is vacuum low-temperature drying, and the drying temperature is 65-80 ℃.
4. Evaporation of mother liquor for preparing potassium-nitrogen composite fertilizer
Neutralizing acidolysis reaction liquid with ammonia water, curing, press-filtering to obtain precipitate, and making mother liquor contain K2SO4And (NH)4)2SO4Etc. and simultaneously contains a small amount of NH4And X, if NaX does not need to be recovered, mixing the mother liquor obtained after the first neutralization for preparing the white carbon black with the mother liquor obtained after the second neutralization for preparing the hydrogen-aluminum oxide, or directly performing double-effect vacuum evaporation, cooling crystallization and filtration respectively to obtain the K-N compound fertilizer. If NaX product is required to be recovered, the mother liquor after the first neutralization and filtration is subjected to single-effect vacuum evaporation to reach a proper concentration, sodium fluoride (NaX) is synthesized by adding calculated and metered sodium carbonate, and then sodium fluoride product is obtained through cooling crystallization and filtration, and the filtrate is subjected to double-effect vacuum evaporation, cooling crystallization, filtration or centrifugal dehydration to obtain the K-N compound fertilizer product.
The relationship between the raw material amount and the output of various products realized in the implementation process of the invention is as follows: every 2 tons of potash feldspar ore, 2 to 2.5 tons of fluorite (95%), 3 to 3.5 tons of industrial sulfuric acid (98%), 2.5 to 3 tons of ammonia water (25 to 28%) and about 50 tons of water are consumed. 1 ton of white carbon black can be produced (wherein, the content of the white carbon black by the gas phase method is 0.65 ton, the content of the white carbon black by the liquid phase method is 0.35 ton), and the content of the silicon dioxide in the white carbon black can reach 98 percent. In addition, 0.3 ton of aluminum hydroxide, 3 ton of potassium-nitrogen compound fertilizer, 0.08 ton of iron oxide red, 0.2 ton of sodium fluoride and 4 ton of gypsum can be produced.
The effective conversion rate of each component in the potash feldspar ore by the process reaches 85-90%; the quality of various produced products respectively meets the requirements of qualified products in corresponding national standards.
The waste liquid generated in the process method contains K2SO4And (NH)4)2SO4The liquid of the substance has low concentration, so that the energy consumption is high if the K-N compound fertilizer is prepared by evaporation crystallization, the cost is not economic, a large water pool can be built, the waste liquid of the liquid is stored in idle time, and the liquid is conveyed to farmers by pipelines to be used as low-concentration liquid potassium-ammonia fertilizer when the liquid is needed in busy farming. If the leakage happens, the environment is affected.
Claims (8)
1. The wet decomposition production process of potassium feldspar is characterized by comprising the following steps of:
1) adding feldspar powder into fluorite powder and a small amount of water, mixing and stirring into paste, gradually adding sulfuric acid, and stirring at 50-80 ℃ for acidolysis reaction to generate silicon-containing gas and solid-phase residue;
2) inputting the silicon-containing gas generated in the step 1) into a Venturi absorber for absorption, adding ammonia water into absorption liquid for neutralization, and washing, drying and crushing the filtered precipitate to obtain fumed silica;
3) filtering and separating the acidolysis solution and the solid-phase residue in the step 1), and washing the solid-phase residue to obtain gypsum;
4) adding ammonia water into the filtered and washed liquid in the step 3) for neutralization, adjusting the pH value to 9-9.5, curing at the temperature of 70-80 ℃, and filtering to obtain a precipitate;
5) adding sulfuric acid into the precipitate obtained in the step 4), reacting, washing with water, filtering, drying and crushing to obtain the liquid-phase white carbon black;
6) adding ammonia water into the filtering and washing liquid obtained in the step 5) for neutralization, curing at the temperature of 70-80 ℃, filtering, washing, drying the filtered precipitate, and crushing to obtain aluminum hydroxide;
7) evaporating the filtrate and the washing liquid in the step 5) or the step 6), cooling, crystallizing and filtering to obtain the K-N compound fertilizer.
2. The wet decomposition production process of potassium feldspar according to claim 1, wherein the wet decomposition production process comprises the following steps: in the step 1), the potash feldspar ore powder, fluorite powder and sulfuric acid are added according to the proportion (in parts by weight) of 1: 1-2: 2-3.
3. The wet decomposition production process of potassium feldspar according to claim 1 or 2, characterized in that: in step 1), the absorption liquid filtered off in step 2) is initially charged and then sulfuric acid is added.
4. The wet decomposition production process of potassium feldspar according to claim 1, wherein the wet decomposition production process comprises the following steps: the curing time in the step 4) and the step 6) is 30-60 minutes.
5. The wet decomposition production process of potassium feldspar according to claim 1, wherein the wet decomposition production process comprises the following steps: the drying in the step 2), the step 5) and the step 6) is vacuum low-temperature drying, and the drying temperature is 65-80 ℃.
6. The wet decomposition production process of potassium feldspar according to claim 1, wherein the wet decomposition production process comprises the following steps: evaporating the filtered liquid in the step 4), adding sodium carbonate for synthesis, cooling for crystallization, and filtering to obtain the sodium fluoride.
7. The wet decomposition production process of potassium feldspar according to claim 1, wherein the wet decomposition production process comprises the following steps: the filtration in the step 2), the step 5) and the step 6) adopts filter pressing.
8. The wet decomposition production process of potassium feldspar according to claim 1, wherein the wet decomposition production process comprises the following steps: the washing in the step 2), the step 5) and the step 6) adopts warm water with the temperature of 40-80 ℃.
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Cited By (9)
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| CN101798095A (en) * | 2010-03-10 | 2010-08-11 | 昊青薪材（北京）技术有限公司 | Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock |
| CN102001691A (en) * | 2010-12-01 | 2011-04-06 | 陈锋 | Process for producing potassium nitrate by decomposing potassium feldspar at low temperature through fluorine-contained acid |
| CN1948228B (en) * | 2006-11-02 | 2011-06-22 | 山东科技大学 | Method of producing potassium fertilizer using waste gypsum to decompose potash feldspar |
| CN102557050A (en) * | 2011-12-20 | 2012-07-11 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
| CN103539148A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Method for preparing molecular sieve by use of potassium feldspar |
| CN103588209A (en) * | 2013-11-01 | 2014-02-19 | 青岛星火化工技术有限公司 | Method for recovery and comprehensive utilization of SiF4 gas |
| CN103708524A (en) * | 2013-12-24 | 2014-04-09 | 贵州远盛钾业科技有限公司 | Method for preparing chemical materials by decomposing potassium-bearing rock by fluorosilicic acid cycling method |
| CN103787421A (en) * | 2013-12-24 | 2014-05-14 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of sylvine-containing rock |
| CN107416845A (en) * | 2017-08-25 | 2017-12-01 | 陕西科技大学 | A kind of method that potassium feldspar produces white silica gel |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1133274A (en) * | 1995-04-13 | 1996-10-16 | 杨冬青 | Method of extracting potassium from potash feldspar |
| CN1072197C (en) * | 1996-03-19 | 2001-10-03 | 化学工业部长沙化学矿山设计研究院 | Wetting decomposition process of potash feldspar ore |
| CN1314628C (en) * | 2004-02-04 | 2007-05-09 | 薛彦辉 | Low temperature decomposition method for potassium feldspar |
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2005
- 2005-09-12 CN CNB2005100194239A patent/CN1318297C/en not_active Expired - Fee Related
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| CN1948228B (en) * | 2006-11-02 | 2011-06-22 | 山东科技大学 | Method of producing potassium fertilizer using waste gypsum to decompose potash feldspar |
| CN101798095A (en) * | 2010-03-10 | 2010-08-11 | 昊青薪材（北京）技术有限公司 | Process for preparing sodium potassium silicate solution by predesiliconizing potassium-rich rock |
| CN102001691A (en) * | 2010-12-01 | 2011-04-06 | 陈锋 | Process for producing potassium nitrate by decomposing potassium feldspar at low temperature through fluorine-contained acid |
| CN102557050A (en) * | 2011-12-20 | 2012-07-11 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
| CN102557050B (en) * | 2011-12-20 | 2013-09-04 | 昆明冶金研究院 | New process for comprehensively utilizing potassium feldspar |
| CN103539148B (en) * | 2013-10-31 | 2015-08-19 | 洛阳氟钾科技股份公司 | Potassium felspar sand is utilized to produce the method for molecular sieve |
| CN103539148A (en) * | 2013-10-31 | 2014-01-29 | 洛阳氟钾科技有限公司 | Method for preparing molecular sieve by use of potassium feldspar |
| CN103588209A (en) * | 2013-11-01 | 2014-02-19 | 青岛星火化工技术有限公司 | Method for recovery and comprehensive utilization of SiF4 gas |
| CN103588209B (en) * | 2013-11-01 | 2015-06-24 | 青岛星火化工技术有限公司 | Method for recovery and comprehensive utilization of SiF4 gas |
| CN103787421A (en) * | 2013-12-24 | 2014-05-14 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of sylvine-containing rock |
| CN103708524B (en) * | 2013-12-24 | 2014-12-17 | 贵州远盛钾业科技有限公司 | Method for preparing chemical materials by decomposing potassium-bearing rock by fluorosilicic acid cycling method |
| CN103787421B (en) * | 2013-12-24 | 2014-12-17 | 贵州远盛钾业科技有限公司 | Comprehensive utilization method of sylvine-containing rock |
| CN103708524A (en) * | 2013-12-24 | 2014-04-09 | 贵州远盛钾业科技有限公司 | Method for preparing chemical materials by decomposing potassium-bearing rock by fluorosilicic acid cycling method |
| CN107416845A (en) * | 2017-08-25 | 2017-12-01 | 陕西科技大学 | A kind of method that potassium feldspar produces white silica gel |
| CN107416845B (en) * | 2017-08-25 | 2019-08-27 | 陕西科技大学 | A kind of method that potassium feldspar produces white silica gel |
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