CN103539184B - Industrial alumen preparation method - Google Patents
Industrial alumen preparation method Download PDFInfo
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- CN103539184B CN103539184B CN201310526328.2A CN201310526328A CN103539184B CN 103539184 B CN103539184 B CN 103539184B CN 201310526328 A CN201310526328 A CN 201310526328A CN 103539184 B CN103539184 B CN 103539184B
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Abstract
The invention provides an industrial alumen preparation method. The industrial alumen preparation method comprises the following steps: 1, fully reacting potassium feldspar powder and ammonium fluoride; 2, adding fluorite powder and concentrated sulfuric acid to a solid mixture obtained after reaction in the step one, wherein solids generated after reaction comprise calcium sulfate, potassium sulfate and aluminium sulfate; step 3, crushing the solids generated after reaction in the step two and dissolving the potassium sulfate and aluminium sulfate in the solids in water; step 4, carrying out filter pressing on mixed liquid obtained after leaching in the step three in a plate-and-frame filter press so as to obtain leaching liquid; step 5, adding the leaching liquid obtained in the step four to a crystallization kettle for carrying out primary concentration and crystallization; and step 6, continuously carrying out concentration and crystallization, and filtering to obtain alumen crystals. The method for preparing industrial alumen by using potassium feldspar, provided by the invention, has the advantages that the alumen production approach is increased, meanwhile the application of potassium feldspar resources is widened, the preparation steps are simple, and the alumen extraction ratio is high.
Description
Technical field
The present invention relates to a kind of preparation method of industrial alum.
Background technology
Alum is used as water purification agent in the industry.Alum can ionize out two metal ion species in water, K
+, Al
3+, wherein Al
3+be easy to hydrolysis, raw jellied aluminium hydroxide, the adsorptive power of alumine hydroxide colloid is very strong, the impurity that can suspend in planar water, and forms precipitation, makes clarification of water.In addition, alum also can be used for preparing aluminium salt, saleratus, paint, tanning material, finings, mordant, papermaking, water-resisting agent etc.Traditional alum by alunite through calcining, extraction, crystallization and obtaining, but alunite is regional at a few at distribution in China, reserves are far away from potassium felspar sand, containing aluminium component in potassium felspar sand, but due to the stability of potassium felspar sand chemical property, ordinary method is difficult to decompose, and therefore, how utilizing potassium felspar sand to prepare industrial alum is current urgent problem.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, thus a kind of preparation method of industrial alum is provided.
To achieve these goals, the technical solution adopted in the present invention is: a kind of preparation method of industrial alum, comprises the following steps:
Step 1, getting feldspar in powder and Neutral ammonium fluoride, is that 1:1.1 ~ 1.2 mix according to mass ratio, and at the temperature of 250 ~ 270 DEG C constant temperature 0.5 ~ 4 hour so that mixed feldspar in powder and Neutral ammonium fluoride fully react;
Step 2, in step 1, add Fluorspar Powder and the vitriol oil in reacted solid mixture, the mass ratio of solid mixture, Fluorspar Powder and the vitriol oil is 1:0.4 ~ 0.5:1, be reaction constant temperature 0.5 ~ 4 hour under the condition of 270 ~ 290 DEG C in temperature, the solid generated after reaction comprises calcium sulfate, potassium sulfate and Tai-Ace S 150;
Step 3, solid step 2 being reacted rear generation are pulverized, and then add in the water of 85 ~ 95 DEG C and leach, temperature keeps 2 hours, and water is 5:1 with the ratio of solid masses, and object is dissolved in water by the potassium sulfate in solid and Tai-Ace S 150;
Step 4, in step 3 leaching after mixed solution in plate-and-frame filter press press filtration to obtain leaching liquid;
Step 5, the leaching liquid of step 4 gained added in crystallization kettle and carry out initial concentration crystallization under the condition of vacuum tightness-0.08MPa and temperature 70 C, and sampling analysis chemical examination, make potassium ion and aluminum ions mol ratio meet 1:1 according to result of laboratory test interpolation moderate amount of sulfuric acid aluminium or potassium sulfate;
Step 6, proceed condensing crystal, filter and obtain alum crystal.
Based on above-mentioned, the reaction of step 1 and step 2 is all carried out in converter.
Based on above-mentioned, the condensing crystal in step 6, adopts first to heat and to be concentratedly stops heating when reaching 50 ~ 60% to alum concentration, and then cooling continues the mode of crystallization, until filter after meeting setting crystallization requirement.
Based on above-mentioned, the mixed gas generated in step 1 and step 2 all absorbs with aqueous ethanolic solution, the silicon tetrafluoride gas in mixed gas and hydrogen fluoride is made to be dissolved in aqueous ethanolic solution, then ammonia solution is carried out to the liquid after absorption, after pH value reaches 8 ~ 9, obtain white carbon black by filter pressing, evaporative crystallization is carried out to filtrate and obtains Neutral ammonium fluoride.
Based on above-mentioned, described ammonia solution is carried out in ammonia solution groove.
Based on above-mentioned, in described aqueous ethanolic solution, the volume ratio of ethanol and aqueous ethanolic solution is 1:10.
The invention provides a kind of method utilizing potassium felspar sand to produce industrial alum, add the production ways of alum, simultaneously, extend the utilization of potassium felspar sand resource, preparation method of the present invention, step is simple, and the extraction yield of alum is high, production efficiency is high, by two-step approach decomposing of potassium feldspar, i.e. step 1 and step 2, substantially increase the rate of decomposition of potassium felspar sand, decrease the consumption of fluorite, Neutral ammonium fluoride can also reclaim Posterior circle utilization simultaneously.
Further, the process of ammonia solution is carried out to the gas collected, can also white carbon black be obtained, decrease the waste of environmental pollution and resource.
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method of the present invention's industry alum.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
The embodiment of a kind of preparation method of industrial alum
Embodiment 1
As shown in Figure 1, comprise the following steps:
Step 1, getting feldspar in powder and Neutral ammonium fluoride, is that 1:1.1 ~ 1.2 mix according to mass ratio, and at the temperature of 250 ~ 270 DEG C constant temperature 0.5 ~ 4 hour so that mixed feldspar in powder and Neutral ammonium fluoride fully react;
Step 2, in step 1, add Fluorspar Powder and the vitriol oil in reacted solid mixture, the vitriol oil is the vitriol oil of 98%, the mass ratio of solid mixture, Fluorspar Powder and the vitriol oil is 1:0.4 ~ 0.5:1, be reaction constant temperature 0.5 ~ 4 hour under the condition of 270 ~ 290 DEG C in temperature, the solid generated after reaction comprises calcium sulfate, potassium sulfate and Tai-Ace S 150;
Step 3, solid step 2 being reacted rear generation are pulverized, and then add in the water of 85 ~ 95 DEG C and leach, temperature keeps 2 hours, and water is 5:1 with the ratio of solid masses, and object is dissolved in water by the potassium sulfate in solid and Tai-Ace S 150;
Step 4, in step 3 leaching after mixed solution in plate-and-frame filter press press filtration to obtain leaching liquid;
Step 5, the leaching liquid of step 4 gained added in crystallization kettle and carry out initial concentration crystallization under the condition of vacuum tightness-0.08MPa and temperature 70 C, and sampling analysis chemical examination, make potassium ion and aluminum ions mol ratio meet 1:1 according to result of laboratory test interpolation moderate amount of sulfuric acid aluminium or potassium sulfate;
Step 6, proceed condensing crystal, filter and obtain alum crystal.
Wherein, the reaction of step 1 and step 2 is all carried out in converter, and solid mixture comprises feldspar in powder, aluminum fluoride and Potassium monofluoride.
A kind of method utilizing potassium felspar sand to produce industrial alum of the present embodiment, adds the production ways of alum, simultaneously, extend the utilization of potassium felspar sand resource, preparation method of the present invention, step is simple, and the extraction yield of alum is high, production efficiency is high, by two-step approach decomposing of potassium feldspar, i.e. step 1 and step 2, substantially increase the rate of decomposition of potassium felspar sand, decrease the consumption of fluorite, Neutral ammonium fluoride can also reclaim Posterior circle utilization simultaneously.
Embodiment 2
As different from Example 1, the condensing crystal in step 6, adopts first to heat and to be concentratedly stops heating when reaching 50 ~ 60% to alum concentration, and then cooling continues the mode of crystallization, until filter after meeting setting crystallization requirement.
Embodiment 3
With embodiment 1,2 unlike, the mixed gas generated in step 1 and step 2 all absorbs with aqueous ethanolic solution, the silicon tetrafluoride gas in mixed gas and hydrogen fluoride is made to be dissolved in aqueous ethanolic solution, then ammonia solution is carried out to the liquid after absorption, after pH value reaches 8 ~ 9, obtain white carbon black by filter pressing, evaporative crystallization is carried out to filtrate and obtains Neutral ammonium fluoride, described ammonia solution is carried out in ammonia solution groove, and in aqueous ethanolic solution, the volume ratio of ethanol and aqueous ethanolic solution is 1:10.
The process of ammonia solution is carried out to the gas collected, can also white carbon black be obtained, decrease the waste of environmental pollution and resource.
Embodiment 4
With embodiment 1-3 unlike, step 1, get feldspar in powder and Neutral ammonium fluoride, be that 1:1.1 mixes according to mass ratio, and at the temperature of 250 DEG C constant temperature 0.5 hour; Fluorspar Powder and the vitriol oil is added in reacted solid mixture in step 1, the mass ratio of solid mixture, Fluorspar Powder and the vitriol oil is 1:0.4:1, be reaction constant temperature 0.5 hour under the condition of 270 DEG C in temperature, the solid generated after reaction comprises calcium sulfate, potassium sulfate and Tai-Ace S 150;
In step 3, solid step 2 being reacted rear generation is pulverized, and then adds in the water of 85 DEG C and leaches.
Embodiment 5
With embodiment 1-4 unlike, step 1, get feldspar in powder and Neutral ammonium fluoride, be that 1:1.15 mixes according to mass ratio, and at the temperature of 260 DEG C constant temperature 2 hours; Fluorspar Powder and the vitriol oil is added in reacted solid mixture in step 1, the mass ratio of solid mixture, Fluorspar Powder and the vitriol oil is 1:0.45:1, be reaction constant temperature 2 hours under the condition of 280 DEG C in temperature, the solid generated after reaction comprises calcium sulfate, potassium sulfate and Tai-Ace S 150;
In step 3, solid step 2 being reacted rear generation is pulverized, and then adds in the water of 90 DEG C and leaches.
Embodiment 6
With embodiment 1-5 unlike, step 1, get feldspar in powder and Neutral ammonium fluoride, be that 1:1.2 mixes according to mass ratio, and at the temperature of 270 DEG C constant temperature 4 hours; Fluorspar Powder and the vitriol oil is added in reacted solid mixture in step 1, the mass ratio of solid mixture, Fluorspar Powder and the vitriol oil is 1:0.5:1, be reaction constant temperature 4 hours under the condition of 290 DEG C in temperature, the solid generated after reaction comprises calcium sulfate, potassium sulfate and Tai-Ace S 150; In step 3, solid step 2 being reacted rear generation is pulverized, and then adds in the water of 95 DEG C and leaches.
Finally should be noted that: above embodiment is only in order to illustrate that technical scheme of the present invention is not intended to limit; Although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the field are to be understood that: still can modify to the specific embodiment of the present invention or carry out equivalent replacement to portion of techniques feature; And not departing from the spirit of technical solution of the present invention, it all should be encompassed in the middle of the technical scheme scope of request of the present invention protection.
Claims (6)
1. a preparation method for industrial alum, is characterized in that comprising the following steps:
Step 1, getting feldspar in powder and Neutral ammonium fluoride, is that 1:1.1 ~ 1.2 mix according to mass ratio, and at the temperature of 250 ~ 270 DEG C constant temperature 0.5 ~ 4 hour so that mixed feldspar in powder and Neutral ammonium fluoride fully react;
Step 2, in step 1, add Fluorspar Powder and the vitriol oil in reacted solid mixture, the mass ratio of solid mixture, Fluorspar Powder and the vitriol oil is 1:0.4 ~ 0.5:1, be reaction constant temperature 0.5 ~ 4 hour under the condition of 270 ~ 290 DEG C in temperature, the solid generated after reaction comprises calcium sulfate, potassium sulfate and Tai-Ace S 150;
Step 3, solid step 2 being reacted rear generation are pulverized, and then add in the water of 85 ~ 95 DEG C and leach, temperature keeps 2 hours, and water is 5:1 with the ratio of solid masses, and object is dissolved in water by the potassium sulfate in solid and Tai-Ace S 150;
Step 4, in step 3 leaching after mixed solution in plate-and-frame filter press press filtration to obtain leaching liquid;
Step 5, the leaching liquid of step 4 gained added in crystallization kettle and carry out initial concentration crystallization under the condition of vacuum tightness-0.08MPa and temperature 70 C, and sampling analysis chemical examination, make potassium ion and aluminum ions mol ratio meet 1:1 according to result of laboratory test interpolation moderate amount of sulfuric acid aluminium or potassium sulfate;
Step 6, proceed condensing crystal, filter and obtain alum crystal.
2. the preparation method of a kind of industrial alum according to claim 1, is characterized in that: the reaction of step 1 and step 2 is all carried out in converter.
3. the preparation method of a kind of industrial alum according to claim 1 and 2, it is characterized in that: the condensing crystal in step 6, adopt first to heat and to be concentratedly stop heating when reaching 50 ~ 60% to alum concentration, then cooling continues the mode of crystallization, until filter after meeting setting crystallization requirement.
4. the preparation method of a kind of industrial alum according to claim 3, it is characterized in that: the mixed gas generated in step 1 and step 2 all absorbs with aqueous ethanolic solution, the silicon tetrafluoride gas in mixed gas and hydrogen fluoride is made to be dissolved in aqueous ethanolic solution, then ammonia solution is carried out to the liquid after absorption, after pH value reaches 8 ~ 9, obtain white carbon black by filter pressing, evaporative crystallization is carried out to filtrate and obtains Neutral ammonium fluoride.
5. the preparation method of a kind of industrial alum according to claim 4, is characterized in that: described ammonia solution is carried out in ammonia solution groove.
6. the preparation method of a kind of industrial alum according to claim 4 or 5, is characterized in that: in described aqueous ethanolic solution, and the volume ratio of ethanol and aqueous ethanolic solution is 1:10.
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| CN103172074A (en) * | 2013-01-17 | 2013-06-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
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| CN103172074A (en) * | 2013-01-17 | 2013-06-26 | 洛阳氟钾科技有限公司 | Process for decomposing potassium feldspar by adopting low-temperature semidry method for comprehensive utilization |
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| 明矾的生产;武炳林;《山西化工》;19871231(第3期);第68页第12行至第23行 * |
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Address after: 471400, Luoyang, Songxian, Henan province Township Po Industrial Agglomeration Area Luoyang fluorine potassium Technology Co., Ltd. Applicant after: LUOYANG POTASSIUM FLUORIDE TECHNOLOGY CO.,LTD. Address before: 471400, Luoyang, Songxian, Henan province Township Po Industrial Agglomeration Area Luoyang fluorine potassium Technology Co., Ltd. Applicant before: Luoyang Fluorine and Potassium Technology Co.,Ltd. Address after: 471400, Luoyang, Songxian, Henan province Township Po Industrial Agglomeration Area Luoyang fluorine potassium Technology Co., Ltd. Applicant after: Luoyang Fluorine and Potassium Technology Co.,Ltd. Address before: 471400, Luoyang, Songxian, Henan province Township Po Industrial Agglomeration Area Luoyang fluorine potassium Technology Co., Ltd. Applicant before: Luoyang Fluoride & Potassium Technology Co.,Ltd. |
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Free format text: CORRECT: APPLICANT; FROM: LUOYANG FLUORIDE + POTASSIUM TECHNOLOGY LTD. TO: LUOYANG FLUORIDE + POTASSIUM TECHNOLOGY CO., LTD. Free format text: CORRECT: APPLICANT; FROM: LUOYANG FLUORIDE + POTASSIUM TECHNOLOGY CO., LTD. TO: LUOYANG FLUORIDE + POTASSIUM TECHNOLOGY COMPANY |
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