CN103539148A - Method for preparing molecular sieve by use of potassium feldspar - Google Patents
Method for preparing molecular sieve by use of potassium feldspar Download PDFInfo
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- CN103539148A CN103539148A CN201310526955.6A CN201310526955A CN103539148A CN 103539148 A CN103539148 A CN 103539148A CN 201310526955 A CN201310526955 A CN 201310526955A CN 103539148 A CN103539148 A CN 103539148A
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Abstract
The invention provides a method for preparing a molecular sieve by use of potassium feldspar. The method comprises the following steps: converting the SiF4 gas obtained by low-temperature decomposition of potassium feldspar and NH4F in a NaOH solution into Na2SiO3 and NaF; meanwhile, leaching the solid residue obtained by the potassium feldspar decomposition to obtain leaching liquid containing K<+>, Al<3+> and SO4<2->; introducing ammonia gas into the leaching liquid to obtain Al(OH)3 precipitate and agricultural compound fertilizer ammonium-potassium sulfate; treating the Al(OH)3 by use of NaOH to obtain NaAlO2; and synthesizing the molecular sieve from NaAlO2 and Na2SiO3 under a hydrothermal condition. By adopting the method provided by the invention to prepare the molecular sieve, the silicon-aluminum ratio and crystal form are adjustable, the agricultural fertilizer ammonium-potassium sulfate and industrial product sodium fluoride are co-produced, comprehensive utilization of the three elements K, Al and Si of the potassium feldspar is realized, and the economic benefit is remarkable.
Description
Technical field
The present invention relates to a kind of method of producing molecular sieve, specifically, related in a kind of industrial production and utilized potassium felspar sand to produce the method for molecular sieve.
Background technology
Molecular sieve, claims again zeolite, is a kind of aluminosilicate of crystal type, because limited by natural resource, nearly all adopts now synthetic.Synthesis of molecular sieve Ji Lv source, silicon source used is determining the quality of technique, product performance and economy.Potassium felspar sand provides silicon, two kinds of resources of aluminium simultaneously, and it is obviously good selection that exploitation potassium felspar sand is produced molecular sieve.In prior art, have a kind of method of utilizing alkaline residue and potassium felspar sand molecular sieve processed, because multiplex fertilizer makes, technological process is difficult to hold, and product performance are not high; Also having a kind of technology is that the former is improved, and adopts soda ash or caustic soda, but still is faced with the problem that technology difficulty is high and constant product quality is poor.If directly adopt purer industrial raw material to carry out large-scale molecular sieve production, obviously economy is bad.
In order to solve the problem of above existence, people are seeking a kind of desirable technical solution always.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, thereby provide a kind of design science, the sial potassium felspar sand that utilizes that when crystal formation is adjustable, element utilization ratio is high, good in economic efficiency to produce the method for molecular sieve.
To achieve these goals, the technical solution adopted in the present invention is: a kind of method of utilizing potassium felspar sand to produce molecular sieve, and preparation process comprises the following steps:
Step 1: potassium felspar sand and NH
4f reaction generates SiF
4gas and contain Al
3+, K
+and F
-residue;
Step 2: to the Al that contains generating in step 1
3+, K
+and F
-residue in add Fluorspar Powder and H
2sO
4, after mixing, reaction generates SiF
4gas and contain Al
3+, K
+, SO
4 2-and CaSO
4residue;
Step 3: by the SiF generating in step 1-2
4gas passes in NaOH solution, obtains the Na containing NaF crystal
2siO
3solution;
Step 4: the resultant in step 3 is purified, from Na
2siO
3in solution, NaF crystal separation is gone out;
Step 5: by the Al that contains generating in step 2
3+, K
+, SO
4 2-and CaSO
4residue in hot water, leach after pulverizing, then press filtration obtains containing K
+, Al
3+, SO
4 2-leaching liquid;
Step 6: add ammoniacal liquor in leaching liquid described in step 5, reaction generates ammonium-potassium sulfate solution and Al (OH)
3precipitation;
Step 7: by the Al filtering out (OH)
3join in NaOH solution, reaction generates NaAlO
2solution, and to this NaAlO
2solution filters purification;
Step 8: by the Na after purifying in step 4
2siO
3naAlO after purifying in solution and step 7
2solution mixes in water, through reaction, obtains molecular sieve work in-process, to described molecular sieve work in-process wash successively, press filtration, dry, obtain molecular sieve finished product.
Based on above-mentioned, the reaction in described step 8 comprises aging and crystallization, and aging temperature is 70 ℃-80 ℃, and digestion time is 1-4 hour; Crystallization temperature is 93 ℃-97 ℃, is advisable with 95 ℃, and crystallization time is 3-4 hour; In described step 8, the silica alumina ratio of two kinds of reactants is 2 ﹕ 1.
Based on above-mentioned, the purification in described step 4 is comprised to centrifugation and the condensing crystal successively carrying out.
Based on above-mentioned, described centrifugation is from Na
2siO
3in solution, NaF crystal separation is gone out to a part, then isolated NaF crystal is washed, is dried, obtain NaF finished product.
Based on above-mentioned, described condensing crystal is from the Na after described centrifugation
2siO
3in solution, isolate NaF crystal, then this NaF crystal is rejoined in the resultant of described step 3, again participate in described step 4; Na through described condensing crystal
2siO
3solution is for participating in the reaction of described step 8.
Based on above-mentioned, in the resultant in described step 1, also comprise ammonia, ammonia absorbs and forms ammoniacal liquor with cold water, and this ammoniacal liquor is for participating in the reaction of step 6.
Based on above-mentioned, in described step 1, potassium felspar sand and NH
4the mass ratio of F is 1 ﹕ (0.4-0.6), and temperature of reaction is 300 ℃-320 ℃, 0.5 hour-2 hours reaction times.
Based on above-mentioned, in described step 2, contain Al
3+, K
+, F
-residue and the mass ratio of Fluorspar Powder and sulfuric acid be that (0.4-0.5) ﹕ (0.7-1), temperature of reaction is 350 ℃-390 ℃ to 1 ﹕, 0.5 hour-2 hours reaction times.
Based on above-mentioned, in described step 5, hot water with contain Al
3+, K
+, SO
4 2-and CaSO
4residue mass ratio be that (3-5) ﹕ 1, temperature is 85 ℃-95 ℃, leaching time (1-3) hour.
The relative prior art of the present invention has outstanding substantive distinguishing features and significant progressive, and specifically, the present invention utilizes potassium felspar sand and NH
4the SiF of F low-temperature decomposition gained
4gas changes into Na in NaOH solution
2siO
3and NaF; Solid slag after potassium felspar sand decomposition simultaneously obtains containing K through leaching
+, Al
3+, SO
4 2-leaching liquid, the logical ammonia of leaching liquid can obtain Al (OH)
3precipitation and agricultural composite fertilizer ammonium-potassium sulfate.With NaOH, process Al (OH)
3can obtain NaAlO
2, NaAlO
2with Na
2siO
3synthesis of molecular sieve under hydrothermal condition.By controlling Na
2siO
3solution and NaAlO
2the proportioning of solution, realizes when crystal formation adjustable of sial, to meet different customer demands, and by-product Agricultural Fertilizer ammonium-potassium sulfate and industrial goods Sodium Fluoride, realize the comprehensive utilization to K-feldspar K, Al, tri-kinds of elements of Si, remarkable in economical benefits.This method of utilizing potassium felspar sand to produce molecular sieve has advantages of design science, sial, and when crystal formation is adjustable, element utilization ratio is high, good in economic efficiency.
Accompanying drawing explanation
Fig. 1 is preparation flow schematic diagram of the present invention.
Embodiment
Below by embodiment, technical scheme of the present invention is described in further detail.
embodiment 1
As shown in Figure 1, a kind of method of utilizing potassium felspar sand to produce molecular sieve, preparation process comprises the following steps:
Step 1: when converter temperature reaches after 350 ℃, proportionally by potassium felspar sand 60Kg and NH
4f(30-40) Kg mixes, and adds in converter feed bin in batches, opens successively batch mixing spiral, star-like blanking device charging, feldspar in powder and NH
4f reacts and generates SiF in converter
4gas and contain Al
3+, K
+and F
-residue.Wherein, potassium felspar sand and NH before reaction
4the mass ratio of F is 1 ﹕ (0.4-0.6), and temperature of reaction is 300 ℃-320 ℃, 0.5 hour-2 hours reaction times.React after half an hour, open discharging spiral, reacted material slag is discharged by stove tail.
Step 2: when converter temperature reaches after 370 ℃, add Fluorspar Powder, Fluorspar Powder added after two minutes opens sulfuric acid charging ball valve, starts sulfuric acid volume pump, according to 48Kg/h:(40-50) ratio of Kg/h adds H
2sO
4react.Contain Al
3+, K
+, F
-residue mix with Fluorspar Powder and sulfuric acid after reaction generate SiF
4gas and contain Al
3+, K
+, SO
4 2-and CaSO
4residue; Contain Al
3+, K
+, F
-residue and the mass ratio of Fluorspar Powder and sulfuric acid be that (0.4-0.5) ﹕ (0.7-1), temperature of reaction is 350 ℃-390 ℃ to 1 ﹕, 0.5 hour-2 hours reaction times.
Step 3: by the SiF generating in step 1-2
4gas passes in the NaOH solution of 1000 liters of 2mol/L, obtains the Na containing NaF crystal
2siO
3solution; The NH generating in step 1-2
3water absorbs.
Step 4: the resultant in step 3 is purified, from Na
2siO
3in solution, NaF crystal separation is gone out.NaF crystal finished product is important industrial goods raw material, has improved potassium felspar sand and has decomposed the economic benefit producing.
Step 5: by the Al that contains generating in step 2
3+, K
+, SO
4 2-and CaSO
4residue in hot water, leach after pulverizing with pulverizer, then in plate-and-frame filter press, carry out press filtration and obtain containing K
+, Al
3+, SO
4 2-leaching liquid; Hot water with contain Al
3+, K
+, SO
4 2-and CaSO
4residue mass ratio be that (3-5) ﹕ 1, temperature is 85 ℃-95 ℃, leaching time (1-3) hour, then naturally cooling.
Step 6: open to stir, add ammoniacal liquor in leaching liquid described in 1000L in step 5, reaction generates ammonium-potassium sulfate solution and Al (OH)
3precipitation; Equal 8 to PH, filter and obtain 25Kg Al (OH)
3precipitation.Institute adds ammonia and Al
3+mol ratio be 3.5 ﹕ 1.Ammonium-potassium sulfate, as by product, is important Agricultural Fertilizer raw material, has obviously improved potassium felspar sand and has decomposed the economic benefit producing.
Step 7: by Al (OH)
3join in NaOH solution, reaction generates NaAlO
2solution.NaOH and Al (OH)
3mol ratio be 1.2 ﹕ 1.According to Na
2o/Al
2o
3=1.34 ratio-dependent NaOH, Al (OH)
3, H
2the consumption of O, the concentration of NaOH is 30%(massfraction).In the NaOH solution of heating, add Al (OH)
3, 115 ℃ are constantly stirred it are fully reacted, obtain NaAlO
2solution, chemical examination sodium aluminate content and to this NaAlO
2solution filters purification.
Step 8: by the Na after purifying in water, mother liquor, step 4
2siO
3naAlO after purifying in solution and step 7
2solution joins in crystallizing kettle successively, adds 10 grams of crystal seeds, if produce 13X type molecular sieve, need to be warming up to 80 ℃, aging 1 hour, then continues to be warmed up to 95 ℃, crystallization 4 hours; If produce 4A type molecular sieve, needing aging temperature is 70 degree, digestion time 4 hours, crystallization temperature 95 degree, 4 hours time.After open kettle cover naturally cooling, obtain molecular sieve work in-process, to described molecular sieve work in-process wash successively, press filtration, dry, obtain molecular sieve finished product.First washing plant is belt filter press, degree of depth washing plate-and-frame filter press, and drying plant is cyclone drying machine.In this step 8, the silica alumina ratio of two kinds of reactants is 2 ﹕ 1.
Silica alumina ratio in molecular sieve and crystal formation can be according to different customer demands and different, and natural mineral composition is fixing, cannot complete this adjusting, so by the step 8 in the present invention, can control Na
2siO
3solution and NaAlO
2the proportioning of solution, realizes the when adjustable object of crystal formation of sial with this.Adjust Na
2o, Al
2o
3, SiO
2, H
2the ratio of O can obtain dissimilar product.
embodiment 2
Embodiment 2 is with the difference of embodiment 1: the purification in described step 4 is comprised to centrifugation and the condensing crystal successively carrying out.
Described centrifugation is from Na in tripod pendulum type batch centrifugal
2siO
3in solution, NaF crystal separation is gone out to a part, then isolated NaF crystal is washed, is dried, obtain NaF crystal finished product.NaF crystal finished product is important industrial goods raw material, has improved potassium felspar sand and has decomposed the economic benefit producing.
Described condensing crystal is in vacuum tightness, for-0.08Mpa, temperature, to be in the crystallization kettle of 70 ℃, from the Na after described centrifugation
2siO
3in solution, isolate NaF crystal crude product, because the NaF crystal crude product through condensing crystal is be not as pure as centrifugalled NaF crystal finished product, so this NaF crystal crude product is rejoined in the resultant of described step 3, again participate in described step 4; Na through described condensing crystal
2siO
3solution is for participating in the reaction of described step 8.
embodiment 3
Embodiment 3 is with the difference of embodiment 2: in the resultant in described step 1, also comprise ammonia, ammonia absorbs and forms ammoniacal liquor with cold water, and this ammoniacal liquor is for participating in the reaction of step 6.After centrifugation, washed in the water of NaF crystal and contained NaF, can be for preparation NaOH solution, this NaOH solution can be used for participating in the reaction of step 3 and step 7.Can find out from above 2, the present invention is recycled waste gas and waste water, participates in production process, has improved the utilization ratio of product in potassium felspar sand decomposition technique in energy-saving and emission-reduction.
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 the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the field are to be understood that: still can modify or part technical characterictic is equal to replacement the specific embodiment of the present invention; 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 that the present invention asks for protection.
Claims (9)
1. utilize potassium felspar sand to produce a method for molecular sieve, it is characterized in that: preparation process comprises the following steps:
Step 1: potassium felspar sand and NH
4f reaction generates SiF
4gas and contain Al
3+, K
+and F
-residue;
Step 2: to the Al that contains generating in step 1
3+, K
+and F
-residue in add Fluorspar Powder and H
2sO
4, after mixing, reaction generates SiF
4gas and contain Al
3+, K
+, SO
4 2-and CaSO
4residue;
Step 3: by the SiF generating in step 1-2
4gas passes in NaOH solution, obtains the Na containing NaF crystal
2siO
3solution;
Step 4: the resultant in step 3 is purified, from Na
2siO
3in solution, NaF crystal separation is gone out;
Step 5: by the Al that contains generating in step 2
3+, K
+, SO
4 2-and CaSO
4residue in hot water, leach after pulverizing, then press filtration obtains containing K
+, Al
3+, SO
4 2-leaching liquid;
Step 6: add ammoniacal liquor in leaching liquid described in step 5, reaction generates ammonium-potassium sulfate solution and Al (OH)
3precipitation;
Step 7: by the Al filtering out (OH)
3join in NaOH solution, reaction generates NaAlO
2solution, and to this NaAlO
2solution filters purification;
Step 8: by the Na after purifying in step 4
2siO
3naAlO after purifying in solution and step 7
2solution mixes in water, through reaction, obtains molecular sieve work in-process, to described molecular sieve work in-process wash successively, press filtration, dry, obtain molecular sieve finished product.
2. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 1, is characterized in that: the reaction in described step 8 comprises aging and crystallization, and aging temperature is 70 ℃-80 ℃, and digestion time is 1-4 hour; Crystallization temperature is 93 ℃-97 ℃, is advisable with 95 ℃, and crystallization time is 3-4 hour; In described step 8, the silica alumina ratio of two kinds of reactants is 2 ﹕ 1.
3. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 1 and 2, is characterized in that: the purification in described step 4 is comprised to centrifugation and the condensing crystal successively carrying out.
4. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 3, is characterized in that: described centrifugation is from Na
2siO
3in solution, NaF crystal separation is gone out to a part, then isolated NaF crystal is washed, is dried, obtain NaF finished product.
5. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 4, is characterized in that: described condensing crystal is from the Na after described centrifugation
2siO
3in solution, isolate NaF crystal, then this NaF crystal is rejoined in the resultant of described step 3, again participate in described step 4; Na through described condensing crystal
2siO
3solution is for participating in the reaction of described step 8.
6. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 1, is characterized in that: in the resultant in described step 1, also comprise ammonia, ammonia absorbs and forms ammoniacal liquor with cold water, and this ammoniacal liquor is for participating in the reaction of step 6.
7. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 1, is characterized in that: in described step 1, and potassium felspar sand and NH
4the mass ratio of F is 1 ﹕ (0.4-0.6), and temperature of reaction is 300 ℃-320 ℃, 0.5 hour-2 hours reaction times.
8. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 1, is characterized in that: in described step 2, contain Al
3+, K
+, F
-residue and the mass ratio of Fluorspar Powder and sulfuric acid be that (0.4-0.5) ﹕ (0.7-1), temperature of reaction is 350 ℃-390 ℃ to 1 ﹕, 0.5 hour-2 hours reaction times.
9. the method for utilizing potassium felspar sand to produce molecular sieve according to claim 1, is characterized in that: in described step 5, hot water with contain Al
3+, K
+, SO
4 2-and CaSO
4residue mass ratio be that (3-5) ﹕ 1, temperature is 85 ℃-95 ℃, leaching time (1-3) hour.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365189A (en) * | 2016-08-29 | 2017-02-01 | 昆明理工大学 | Comprehensive utilization method of silicon residue soil |
| CN109261349A (en) * | 2018-08-31 | 2019-01-25 | 贺州市骏鑫矿产品有限责任公司 | A kind of purification method of whitening of albite |
| CN112320820A (en) * | 2020-10-27 | 2021-02-05 | 贵州省化工研究院 | Method for producing high-purity sodium fluoride by utilizing fluosilicic acid in phosphoric acid |
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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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| US6451282B1 (en) * | 1997-10-28 | 2002-09-17 | SIKLOSI PéTER | Process for production of zeolites from raw materials containing alkali alumino hydro-silicates |
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| CN112320820A (en) * | 2020-10-27 | 2021-02-05 | 贵州省化工研究院 | Method for producing high-purity sodium fluoride by utilizing fluosilicic acid in phosphoric acid |
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