CN103922363B - A kind of take pyrite tailing as the method that 4A zeolite prepared by raw material - Google Patents
A kind of take pyrite tailing as the method that 4A zeolite prepared by raw material Download PDFInfo
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- CN103922363B CN103922363B CN201410178446.3A CN201410178446A CN103922363B CN 103922363 B CN103922363 B CN 103922363B CN 201410178446 A CN201410178446 A CN 201410178446A CN 103922363 B CN103922363 B CN 103922363B
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Abstract
The invention discloses a kind of is the method that 4A zeolite prepared by raw material with pyrite tailing, and belong to chemical field, its step comprises: after pulverizing pyrite tailing, formulation content is the slip of 20 ~ 30%; CuSO is added respectively in slip
4solution, butyl xanthate, pine camphor oil, then filtering drying is levigate; Then add mixed acid solution, after fully stirring, to dry by clean water and levigate; After 620 ~ 650 DEG C of temperature lower calcination 2 ~ 4h, add NaOH solution and at 50 ~ 60 DEG C constant temperature stir 2 ~ 5h; 2 ~ 5h is reacted at 90 ~ 95 DEG C, centrifugal, dry, namely obtain 4A zeolite product.Adopt present method that pyrite tailing can be adopted to prepare 4A zeolite as raw material, thus effective recycling has been carried out to pyrite tailing, decrease pyrite tailing to the cost reducing 4A zeolite raw materials while environment.
Description
Technical field
The present invention relates to chemical field, particularly a kind of take pyrite tailing as the method that 4A zeolite prepared by raw material.
Background technology
4A zeolite is a kind of hydrated aluminosilicate-sodium silicoaluminate crystal, the aluminosilicate crystals of English SodiumAlumino-Silicate system by name synthetic, its chemical formula Na
12[AlO
2(SiO
2)]
1227H
2o, belongs to NaA type zeolite.For the synthesis of 4A zeolite, prior synthesizing method is chemical method, namely with the method that water glass, aluminium hydroxide, caustic soda are raw water thermal synthesis, and the method steady quality, but high cost.Utilize raw mineral materials to synthesize `4A zeolite can reduce costs, have Activated, swelling local method, kaolin method and coal gangue method etc. at present.Wherein kaolin method, utilize kaolin silica alumina ratio and the basically identical feature of 4A zeolite, be translated into the metakaolinite with reactive behavior, and in the caustic soda aqueous solution, carry out hydrothermal crystallization conversion reaction and make zeolite, the method technique is simple, do not need supplementary silicon source and aluminium source, there is lower-cost feature.In kaolin method synthesis 4A zeolite, material choice is very important, strictly will control existence and the content of impurity in kaolin, usually adopt high grade kaolinite.Because impurity can have a strong impact on the structure (as crystalline structure, aperture etc.) of the finished product, physical properties (as color and luster, particle diameter etc.) and chemical property (adsorptivity and ion exchangeable etc.), make the finished product can not reach the requirement of 4A zeolite.
Essential mineral pyrite (the FeS of sulfurous iron ore
2), be a kind of important minerals commonly used in chemical industry raw material, mainly for the manufacture of sulfuric acid.Part is used for industrial chemicals to produce sulphur and various sulfocompounds etc.The said pyrite tailing of this patent refer to exploit out while exploitation sulfurous iron ore with the kaolinite matter clay pit of pyrite.Sulfurous iron ore is after selecting pyrite, and rest part just becomes mine tailing, is called pyrite tailing.Comparatively greatly, essential mineral consists of kaolinite for the mineral composition of pyrite tailing and chemical composition ranges fluctuation, the pyrite etc. also containing a small amount of nakrite, Wingdale, anatase octahedrite and be not selected.The Exemplary chemical of the said pyrite tailing of this patent consists of (weight percent) SiO
230 ~ 52%, Al
2o
325 ~ 40%, CaO0.2 ~ 2.0%, Fe
2o
30.6 ~ 19%, TiO
20.5 ~ 7.0%, SO
30.5 ~ 4.5%, other impurity composition 1 ~ 5%.Although the main mineral constituent of visible pyrite tailing is kaolinite, but compared with general kaolinite, the chemical component fluctuation scope of pyrite tailing is large, titanium content is general higher, add pyritous symbiosis, the union dyeing of organic matter and fixed carbon and pyritous partial surface oxidation, make that impurity in pyrite tailing is many and content is high, be difficult to directly be applied.Therefore, in China Pyrite Mine Area, pyrite tailing can not be utilized for a long time, is deposited in ground or gully, causes serious environmental pollution.
Also just because of the compositing characteristic of above-mentioned pyrite tailing, when traditional kaolin method synthesis 4A zeolite, pyrite tailing is that 4A zeolite synthesis is carried out in the requirement do not met as raw material, and namely pyrite tailing adopts existing technique can not for the synthesis of 4A zeolite.
Summary of the invention
For the problems referred to above, the object of this invention is to provide a kind of pyrite tailing that adopts is the method that 4A zeolite prepared by raw material, to recycle pyrite tailing.
To achieve these goals, the present invention adopts following technical scheme: a kind of is the method that 4A zeolite prepared by raw material with pyrite tailing, comprises the following steps:
(1), after pulverizing pyrite tailing, the slip that solid masses percentage composition is 20 ~ 30% is mixed with;
(2) described slip adjust ph to 8 ~ 9 step (1) obtained, after stirring, add the CuSO that 4 ~ 5L mass concentration is 5% in slip per ton
4solution, after stirring, adds butyl xanthate 150 ~ 250 grams in slip per ton, after stirring, then in slip per ton, adds 120 ~ 200 grams of pine camphor oils, after stirring, scrapes filtering drying after foam-expelling, and levigate to crossing 200 mesh sieves, obtains a powder;
(3) add acid solution in the powder obtained in step (2), the ratio added adds 3.3 ~ 3.8L acid solution for a powder described in per kilogram, heats to 58 ~ 62 DEG C, after abundant stirring, be washed till pH to 5 ~ 6 with clear water, oven dry is also levigate to crossing 200 ~ 500 mesh sieves, obtains secondary powder;
(4) secondary powder that will obtain through step (3) is after 620 ~ 650 DEG C of temperature lower calcination 2 ~ 4h, add the NaOH solution that volumetric molar concentration is 2.8 ~ 4.0mol/L, the ratio added is for adding NaOH solution described in 5L in per kilogram secondary powder, and at 50 ~ 60 DEG C, constant temperature stirs 2 ~ 5h, obtains middle product;
(5) 2 ~ 5h will be reacted by product in the middle of step (4) gained at 90 ~ 95 DEG C, obtain work in-process;
(6) will be centrifugal by step (5) gained work in-process, dry, namely obtain 4A zeolite product.
Present method and pyrite tailing that foreign matter content high complicated with impurity component prepares 4A zeolite for raw material, in order to prepare the 4A zeolite of qualified even high-quality, above-mentioned steps (1)-(3) carry out composition adjustment to pyrite tailing, comprise the silica alumina ratio in the content and adjustment raw material reducing impurity, concrete:
In step (1), after pyrite tailing fragmentation, be beneficial to the removal of follow-up impurity;
In step (2), because pyrite surface electric charge is just, easily by xanthate anionoid adsorption of collector, and pine camphor oil is as pore forming material, is conducive to the surface tension reducing the aqueous solution, makes the air be filled with in water be easy to disperse and become bubble and stabilise bubbles.Pine camphor oil and xanthate is united is adsorbed in mineral particle surface, makes ore particle float, thus the effective impurity such as removing pyrite, and the existence of copper sulfate can suppress unsulfided to be adsorbed;
In step (3), the iron cpd adopting acid solution to make ferric ion generate solubility enters solution, thus deironing further, and can remove portion titanium and adjustment silica alumina ratio.
After adopting the method process of step (1)-(3), composition and the high grade kaolinite of the secondary powder obtained are similar, then adopt and are similar to the synthesis that kaolin method carries out 4A zeolite, concrete:
In step (4), the object of calcining mine tailing is after treatment that activation of kaoline is become metakaolin, and its reaction formula is: Al
2si
2o
5(OH)
4→ Al
2si
2o
7+ 2H
2o.Active metakaolin after calcining under optimal temperature with NaOH solution ageing, its objective is and make it be transformed into uniform Edge by Aluminosilicate Sol-gel gradually, formed transform molecular sieve precursor, for follow-up crystallization process lays the foundation.The reaction formula of this process is:
6(Al
2O
3·2SiO
2)+12NaOH+21H
2O→Na
12[(AlO
2)(SiO
2)]
12·27H
2O。
In step (4), have employed compared with the kaolin method of routine, lower calcining temperature 620 ~ 650 DEG C, the calcining temperature of conventional kaolin method is generally 750-850 DEG C, and this all has benefited from the pretreatment process that have employed the distinctive removal of impurities of the present invention and composition adjustment; Lower calcining temperature, on the one hand can save energy, can extend the duration of service of calciner on the other hand.
As preferred technical scheme: in step (1), pulverize pyrite tailing to crossing 200 ~ 500 mesh sieves.The 4A zeolite whiteness of synthesis is relevant with the granularity of calcium ion-exchanged amount and raw material, general raw material pulverizing fine size, is conducive to improving whiteness and calcium ion-exchanged amount.
As preferred technical scheme: in step (2), during adjust ph, mass percentage concentration is adopted to be the Na of 10%
2cO
3solution.
As preferred technical scheme: in step (3), described acid solution is mixed acid solution, described mixed acid solution be with mass concentration be 25% ~ 35% sulfuric acid and hydrochloric acid soln for component, and 1:1 is formulated by volume.If only use HCl treatment pyrite tailing, de-ferrous effect is better, but for the higher mine tailing of titaniferous, but effectively can not improve whiteness; Use vitriolization pyrite tailing then can remove the titanium of a part while the iron of a removing part.Adopt " sulfuric acid+hydrochloric acid " to process pyrite tailing, can insoluble compound wherein be changed into soluble compounds, and be separated with kaolin, effectively remove iron contamination, and partly can remove titanium contained in kaolin, improve kaolin whiteness.In addition, kaolin stability is in mineral acid better, through persalt or vitriolization, only has little Al
2o
3be dissolved, use mixing acid process kaolin to be more conducive to adjusting kaolinic silica alumina ratio.
In sum, owing to have employed technique scheme, the invention has the beneficial effects as follows: adopt method of the present invention, pyrite tailing can be adopted to prepare 4A zeolite as raw material, thus effective recycling has been carried out to pyrite tailing, decrease pyrite tailing to the cost reducing 4A zeolite raw materials while environment; And the crystalline structure of the 4A zeolite prepared, aperture, physical properties (as color and luster, particle diameter etc.) and chemical property (adsorptivity and ion exchangeable etc.), can reach the requirement of 4A zeolite.If color and luster is white, whiteness is 85-90%, and calcium ion-exchanged amount reaches 300-340mgCaCO
3/ g.The pH value of 4A zeolite is 10-11.2.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the 4A zeolite that the embodiment of the present invention 1 obtains;
Fig. 2 is the XRD figure of the 4A zeolite that the embodiment of the present invention 2 obtains;
Fig. 3 is the XRD figure of the 4A zeolite that the embodiment of the present invention 3 obtains;
In Fig. 1-3, X-coordinate is diffraction angle " 2-theta ", and unit is " degree "; Ordinate zou is " intensity ", and unit is " a.u ".
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
Pyrite tailing that the present embodiment uses takes from southern Sichuan enterprise pyrite tailing storehouse, is that enterprise piles up the mine tailing got off in decades for a long time, and because production technology level is originally low, therefore iron in this mine tailing, titanium, sulphur content are all very high.Its chemical component weight per-cent is: SiO
240.89%, A1
2o
333.87%, CaO3.97%, TiO
25.01%, Fe
2o
36.09%, K
2o0.18%, SO
39.55%, other are 0.43% years old.This pyrite tailing is used to prepare the processing step of 4A zeolite as follows:
(1) with ball mill by levigate for pyrite tailing to crossing after 325 mesh sieves, take 300g preparation of powder and become solid masses percentage composition be the slip of 25% and be placed in certain container;
(2) in the slip obtained by step (1), the Na that mass concentration is 10% is added
2cO
3solution, adjust ph to 8 ~ 9, after stirring 3min, in slip per ton, add 5 mass per liter concentration is the CuSO of 5%
4solution, after stirring 3min, adds 250 grams of butyl xanthates in slip per ton, after stirring 3min, then in slip per ton, adds 200 grams of pine camphor oils; After stirring for 180 seconds, start to scrape bubble; After this operation repeats to do 3 road flotation, suction filtration is dried, and levigate to crossing 200 mesh sieves, obtains a powder;
(3) respectively prepare mass concentration be 30% sulfuric acid and mass concentration be 30% hydrochloric acid soln;
(4) with the sulfuric acid prepared by step (3) and hydrochloric acid soln by volume 1:1 be mixed with mixed acid solution;
(5) mixed acid solution will prepared by step (4) is by 3.5L/kg
powderratio join in the powder obtained by step (2), heat to 58 DEG C, fully stir after 1 hour, be washed till pH to 5-6 with clear water, dry and levigately cross mesh sieves to 325, obtain secondary powder;
(6) secondary powder that will obtain through step (5) after 620 DEG C of temperature lower calcination 4h, by 5L/kg
powderratio add the NaOH solution of volumetric molar concentration 2.8mol/L, and at 55 DEG C, constant temperature stirs 4h, obtains middle product;
(7) reactor will be put into by product in the middle of step (6) gained, and at 90 DEG C, react 2h, obtain work in-process;
(8) by step (7) gained work in-process centrifugal drying, 4A zeolite product will namely be obtained.
Prepared product is 4A zeolite, is white cubic crystal, nontoxic, tasteless, non-corrosiveness.Water insoluble and organic solvent, can be dissolved in strong acid and highly basic, pH value is 10, and its stable range is 5 ~ 12; Median size is 1.48 μm, and size-grade distribution≤4 μm account for 85.6%.X-ray powder diffraction (XRD) material phase analysis as shown in Figure 1, in the XRD spectra of synthetic product except there is a small amount of unknown dephasign diffraction peak, the standard diagram of other diffraction peak and 4A zeolite is completely the same, shows that product crystalline phase is 4A zeolite synthesized by example 1 technique used.Its calcium ion-exchanged amount is 300.48mgCaCO
3/ g, whiteness is 87%.
Embodiment 2
Pyrite tailing that the present embodiment uses takes from southern Sichuan enterprise pyrite tailing storehouse, and its chemical component weight per-cent is: SiO
245.90%, A1
2o
337.05%, CaO1.98%, TiO
25.03%, Fe
2o
33.91%, K
2o0.56%, SO
31.27%, other are 4.29% years old.This pyrite tailing is used to prepare the processing step of 4A zeolite as follows:
(1) with ball mill by levigate for pyrite tailing to crossing after 325 mesh sieves, take 300g preparation of powder and become solid masses percentage composition be the slip of 30% and be placed in certain container;
(2) in the slip obtained by step (1), the Na that mass concentration is 10% is added
2cO
3solution, adjust ph to 8 ~ 9, after stirring 2.5min, in slip per ton, add 4.5 mass per liter concentration is the CuSO of 5%
4solution, after stirring 2.5min, adds 150 grams of butyl xanthates in slip per ton, after stirring 1min, then in slip per ton, adds 160 grams of pine camphor oils; After stirring for 90 seconds, start to scrape bubble; After this operation repeats to do 3 road flotation, suction filtration is dried, and levigate to crossing 200 mesh sieves, obtains a powder;
(3) respectively prepare mass concentration be 35% sulfuric acid and mass concentration be 35% hydrochloric acid soln;
(4) with the sulfuric acid prepared by step (3) and hydrochloric acid soln by volume 1:1 be mixed with mixed acid solution;
(5) mixed acid solution will prepared by step (4) is by 3.8L/kg
powderratio join in the powder obtained by step (2), heat to 62 DEG C, fully stir after 1 hour, be washed till pH to 5-6 with clear water, dry and levigately cross mesh sieves to 200, obtain secondary powder;
(6) secondary powder that will obtain through step (5) after 650 DEG C of temperature lower calcination 4h, by 5L/kg
powderratio add the NaOH solution of volumetric molar concentration 4.0mol/L, and at 60 DEG C, constant temperature stirs 5h, obtains middle product;
(7) reactor will be put into by product in the middle of step (6) gained, and at 95 DEG C, react 5h, obtain work in-process;
(8) by step (7) gained work in-process centrifugal drying, 4A zeolite product will namely be obtained.
Prepared product is 4A zeolite, is white cubic crystal, nontoxic, tasteless, non-corrosiveness.Water insoluble and organic solvent, can be dissolved in strong acid and highly basic, pH value is 11, and its stable range is 5-12; Median size 2.24 μm, size-grade distribution≤4 μm account for 85.48%.X-ray powder diffraction (XRD) material phase analysis as shown in Figure 2, in the XRD spectra of synthetic product except there is a small amount of unknown dephasign diffraction peak, the standard diagram of other diffraction peak and 4A zeolite is completely the same, show that product crystalline phase is 4A zeolite synthesized by example 2 technique used, and due to Synthesis of 4 A-type Zeolite by Hydrothermal crystallization time longer, crystal growth is perfect.This synthetic product whiteness is 87%, and its calcium ion-exchanged amount is 320.64mgCaCO
3/ g.
Embodiment 3
The present embodiment use pyrite tailing to take from the flotation cell of the small-sized heavy floating choosing of southern Sichuan enterprise, its chemical component weight per-cent is: SiO
238.41%, A1
2o
332.40%, CaO3.02%, TiO
24.01%, MgO0.76%, Fe
2o
31.91%, Na
2o0.16%, K
2o0.35%, SO
30.92%, other are 0.80% years old.This pyrite tailing is used to prepare the processing step of 4A zeolite as follows:
(1) with ball mill by levigate for pyrite tailing to crossing after 200 mesh sieves, take 300g preparation of powder and become solid masses percentage composition be the slip of 20% and be placed in certain container;
(2) in the slip obtained by step (1), the Na that mass concentration is 10% is added
2cO
3solution, adjust ph to 8 ~ 9, after stirring 2min, in slip per ton, add 4 mass per liter concentration is the CuSO of 5%
4solution, after stirring 2min, adds 200 grams of butyl xanthates in slip per ton, after stirring 1.5min, then in slip per ton, adds 120 grams of pine camphor oils; After stirring for 30 seconds, start to scrape bubble; After this operation repeats to do 3 road flotation, suction filtration is dried, and levigate to crossing 200 mesh sieves, obtains a powder;
(3) respectively prepare mass concentration be 25% sulfuric acid and mass concentration be 25% hydrochloric acid soln;
(4) with the sulfuric acid prepared by step (3) and hydrochloric acid soln by volume 1:1 be mixed with mixed acid solution;
(5) mixed acid solution will prepared by step (4) is by 3.36L/kg
powderratio join in the powder obtained by step (2), heat to 60 DEG C, fully stir after 1 hour, be washed till pH to 5-6 with clear water, dry and levigately cross mesh sieves to 325, obtain secondary powder;
(6) secondary powder that will obtain through step (5) after 630 DEG C of temperature lower calcination 3h, by 5L/kg
powderratio add the NaOH solution of volumetric molar concentration 3.0mol/L, and at 50 DEG C, constant temperature stirs 3h, obtains middle product;
(7) reactor will be put into by product in the middle of step (6) gained, and at 92 DEG C, react 3h, obtain work in-process;
(8) by step (7) gained work in-process centrifugal drying, 4A zeolite product will namely be obtained.
Prepared product is 4A zeolite, is white cubic crystal, nontoxic, tasteless, non-corrosiveness.Water insoluble and organic solvent, can be dissolved in strong acid and highly basic, pH value is 11.2, and its stable range is 6-13, and median size is 2.11 μm, and size-grade distribution≤4 μm account for 89.84%.X-ray powder diffraction (XRD) material phase analysis as shown in Figure 3, in the XRD spectra of synthetic product except there is a small amount of unknown dephasign diffraction peak, the standard diagram of other diffraction peak and 4A zeolite is completely the same, shows that product crystalline phase is 4A zeolite synthesized by example 3 technique used.This synthetic product whiteness is 90%, and calcium ion-exchanged amount is 330.68mgCaCO
3/ g.
Claims (3)
1. be the method that 4A zeolite prepared by raw material with pyrite tailing, it is characterized in that, comprise the following steps:
(1), after pulverizing pyrite tailing, the slip that solid masses percentage composition is 20 ~ 30% is mixed with;
(2) described slip adjust ph to 8 ~ 9 step (1) obtained, after stirring, add the CuSO that 4 ~ 5L mass concentration is 5% in slip per ton
4solution, after stirring, adds butyl xanthate 150 ~ 250 grams in slip per ton, after stirring, then in slip per ton, adds 120 ~ 200 grams of pine camphor oils, after stirring, scrapes filtering drying after foam-expelling, and levigate to crossing 200 mesh sieves, obtains a powder;
(3) add acid solution in the powder obtained in step (2), the ratio added adds 3.3 ~ 3.8L acid solution for a powder described in per kilogram, heats to 58 ~ 62 DEG C, after abundant stirring, be washed till pH to 5 ~ 6 with clear water, oven dry is also levigate to crossing 200 ~ 500 mesh sieves, obtains secondary powder;
(4) secondary powder that will obtain through step (3) is after 620 ~ 650 DEG C of temperature lower calcination 2 ~ 4h, add the NaOH solution that volumetric molar concentration is 2.8 ~ 4.0mol/L, the ratio added is for adding NaOH solution described in 5L in per kilogram secondary powder, and at 50 ~ 60 DEG C, constant temperature stirs 2 ~ 5h, obtains middle product;
(5) 2 ~ 5h will be reacted by product in the middle of step (4) gained at 90 ~ 95 DEG C, obtain work in-process;
(6) will be centrifugal by step (5) gained work in-process, dry, namely obtain 4A zeolite product;
In step (3), described acid solution is mixed acid solution, described mixed acid solution be with mass concentration be 25% ~ 35% sulfuric acid and hydrochloric acid soln for component, and 1:1 is formulated by volume.
2. a kind of is according to claim 1 the method that 4A zeolite prepared by raw material with pyrite tailing, it is characterized in that: in step (1), pulverizes pyrite tailing to crossing 200 ~ 500 mesh sieves.
3. a kind of is according to claim 1 the method that 4A zeolite prepared by raw material with pyrite tailing, it is characterized in that: in step (2), adopts mass percentage concentration to be the Na of 10% during adjust ph
2cO
3solution.
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| Title |
|---|
| 王德清 等.高岭石型硫铁矿烧渣合成磁性4A沸石及其表征.《材料导报B:研究篇》.2014,第28卷(第3期),第119-123页. * |
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