CN104556097A - Method for preparing hydrotalcite-like compounds and zeolites by using blast furnace slag - Google Patents
Method for preparing hydrotalcite-like compounds and zeolites by using blast furnace slag Download PDFInfo
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- CN104556097A CN104556097A CN201510018368.5A CN201510018368A CN104556097A CN 104556097 A CN104556097 A CN 104556097A CN 201510018368 A CN201510018368 A CN 201510018368A CN 104556097 A CN104556097 A CN 104556097A
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Abstract
The invention discloses a method for preparing hydrotalcite-like compounds and zeolites by using blast furnace slag. The method comprises the following process flows: crushing the blast furnace slag, gelating hydrochloric acid, stirring at constant temperature and filtering; adding a sodium hydroxide solution into the filtrate to adjust the pH, stirring at constant temperature, aging, filtering, washing, drying and grinding to obtain the hydrotalcite-like compounds; and washing, drying and grinding the gel, adding the sodium hydroxide solution to adjust the pH, stirring at room temperature, adding an aluminum-containing solution, stirring at constant temperature, aging, filtering, washing and drying to obtain the zeolites. The method for preparing the hydrotalcite-like compounds and the zeolites by using blast furnace slag provided by the invention fully utilizes a blast furnace slag raw material to synthesize the hydrotalcite-like compounds and zeolites. The market prices of the hydrotalcite-like compounds and the zeolites are higher than that of the blast furnace slag, so that the utilization range of the blast furnace slag is greatly improved, the additional value of blast furnace slag utilization is increased and the economic profit of iron and steel enterprises is improved. The method has a good market application prospect.
Description
Technical field
The invention belongs to the application technology as the second resource field of Industrial Solid Waste, relate to the utilization of blast furnace slag, be specifically related to a kind of method utilizing blast furnace slag to prepare houghite and zeolite.
Background technology
According to the data presentation that world steel association announces, within 2012, global pig iron output is 1,100,000,000 tons, and the country that wherein output is the highest is China, and the output of 2012 1 year is up to 6.5 hundred million tons.In blast furnace ironmaking process, even if calculate according to the slag ratio of 300Kg, the output of blast-furnace slag is also up to nearly 200,000,000 tons.These blast-furnace slags how are utilized to become the focus of people's concern gradually efficiently.What the blast furnace slag treating process of present stage all adopted substantially is flush slag technique, and the product obtained is substantially for manufacture of cement, but the blast furnace granulated slag being used as cement producting material almost has no profit can say.
Houghite (Hydrotalcite-Like Compounds is called for short HTLCs) belongs to layered di-hydroxyl composite metal oxidate (Layered Double Hydroxide is called for short LDH).HTLCs can use general formula [M (II)
1-xm (III)
x(OH)
2]
x+[A
x/n n-] mH
2o represents, wherein M
2+and M
3+represent divalence and Tricationic on layer respectively, A
n-for interlayer anion, x=M
3+/ (M
2++ M
3+), only in the scope of 0.2<x<0.34, just can synthesize hydrotalcite that is pure, high-crystallinity.The most basic structural unit of zeolite is SiO
4and AlO
4tetrahedron, shares Sauerstoffatom in the mode of oxo bridge key between adjacent tetrahedron.What be positioned at tetrahedron center is Si atom or Al atom, and tetrahedron each summit place is Sauerstoffatom, Si atom or Al atom respectively with oxygen atoms bond.This combination makes it on three-dimensional, form the inorganic polymeric that has ordered structure.
Summary of the invention
The main component of blast furnace slag is CaO, MgO, SiO
2, Al
2o
3, belong to phyllosilicate material, its chemical constitution and natural crystal, silicate cement are similar.Wherein, the cation ratio of houghite divalence and trivalent is between 2 ~ 5, and (the Ca+Mg)/Al ≈ 3 in blast furnace slag, be applicable to very much preparing houghite; And the SiO extracted
2can be used to prepare zeolite.
In view of this, the object of the present invention is to provide a kind of method utilizing blast furnace slag to prepare houghite and zeolite, fully effectively to utilize the composition of blast furnace slag.
Concrete, the invention provides following technical scheme:
The method utilizing blast furnace slag to prepare houghite and zeolite of the present invention, comprises the steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, stir under boiling water bath, until the silicon part gel in blast furnace slag, be 50 ~ 60ml relative to the add-on of every gram of blast furnace slag hydrochloric acid, described concentration of hydrochloric acid is 3mol/L;
Preferably, in massfraction, described blast furnace slag comprises following compositions: SiO
2be 35 ~ 40%, CaO be 35 ~ 40%, MgO be 5 ~ 15%, Al
2o
3be 5 ~ 15%, surplus is trace ingredients.
(2) filter, respectively filtrate and gel for subsequent use;
(3) in the filtrate of step (2) gained, dripping sodium hydroxide solution, is 9.5 ~ 13.5 to pH value, forms suspension liquid;
Preferably, described concentration of sodium hydroxide solution is 2 ~ 4mol/L.
(4) suspension liquid will obtained in step (3), stirs 0.5 ~ 2h in 60 ~ 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, ageing 12 ~ 24h at 60 ~ 100 DEG C;
(5) solution of step (4) ageing is filtered, and washed screening is to PH to less than 8, obtains houghite after drying;
(6) by after the gel repetitive scrubbing that obtains in step (2), dry, grinding, obtains silica flour;
(7) add sodium hydroxide solution violent stirring in the silica flour obtained to step (6), form uniform suspension liquid;
Preferably, described concentration of sodium hydroxide solution is 2 ~ 4mol/L.
(8) in the suspension liquid obtained to step (7), titration is containing aluminum solutions, and stirs 0.5 ~ 1h;
Preferably, described is sodium aluminate solution or potassium aluminate solution containing aluminum solutions.
(9) moved in Hydrothermal Synthesis still by the suspension liquid in step (8), bath temperature is 80 ~ 120 DEG C of ageing 3 ~ 8h, and then filtration washing drying obtains zeolite.
The method utilizing blast furnace slag to prepare houghite and zeolite provided by the invention, take full advantage of blast furnace slag raw material, synthesis hydrotalcite-like material and zeolite, the market value of houghite and zeolite is higher than the price of blast furnace slag, what substantially increase blast furnace slag utilizes scope, add the added value of blast furnace utilization, improve the economic profit of iron and steel enterprise, there is good market application foreground.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing for the present invention in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the process flow sheet utilizing blast furnace slag to prepare houghite and zeolite provided by the invention;
Fig. 2 is that in embodiment 1 ~ 3, digestion time is 12h, the XRD figure of houghite during different PH;
Fig. 3 is that in embodiment 4 ~ 6, digestion time is 18h, the XRD figure of houghite during different PH;
Fig. 4 is that in embodiment 7 ~ 9, digestion time is 24h, the XRD figure of houghite during different PH;
The SEM figure of houghite when Fig. 5 is different ageing and pH value in embodiment 1 ~ 9;
Fig. 6 is the XRD figure of different ageing zeolite in embodiment 10 ~ 12;
Fig. 7 is the SEM figure of different ageing zeolite in embodiment 10 ~ 12.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is described in detail.
As shown in Figure 1, the method utilizing blast furnace slag to prepare houghite and zeolite provided by the invention, its technical process comprises: the first stage, pulverizes, salt acid gel, and constant temperature stirs, and filters; Subordinate phase, filtrate hydro-oxidation sodium solution, constant temperature stirs, ageing, filters, and washing is dry, and grinding, obtains houghite; Phase III, gel detergent, dry, grinding, hydro-oxidation sodium solution, stirring at room temperature, adds sodium aluminate solution, and constant temperature stirs, ageing, filters, and washing is dry, obtains zeolite.
Use blast furnace slag that certain Steel Plant produces as main raw material in the present invention, other raw material added is hydrochloric acid, sodium hydroxide, sodium aluminate, deionized water etc., and the houghite prepared at different temperature and PH condition has different character.
The blast furnace slag used in the present invention comprises following compositions: SiO
2be 35 ~ 40wt%, CaO be 35 ~ 40wt%, MgO be 5 ~ 15wt%, Al
2o
3be 5 ~ 15wt%, FeO, MnO, K
2o, Na
2o trace.
The one-tenth that table 1 gives the blast furnace slag used in the embodiment of the present invention is grouped into.
Table 1 blast furnace slag main component
Below provide in the present invention the specific embodiment using blast furnace slag to prepare houghite and zeolite.
Embodiment 1
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=9.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 12h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a large amount of dephasigns.
Embodiment 2
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=11.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 12h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a small amount of dephasign.
Embodiment 3
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=13.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 12h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a small amount of dephasign.
Embodiment 4
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=9.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 18h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a large amount of dephasigns.
Embodiment 5
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=11.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 18h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a small amount of dephasign.
Embodiment 6
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=13.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 18h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a small amount of dephasign.
Embodiment 7
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=9.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 24h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a large amount of dephasigns.
Embodiment 8
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=11.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 24h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a small amount of dephasign.
Embodiment 9
What the present embodiment provided utilizes blast furnace slag to prepare the method for houghite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) to the sodium hydroxide solution of titration 3mol/L in filtrate, to PH=13.5, suspension liquid is formed;
(4) suspension liquid stirs 1h in 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, at 65 DEG C of ageing 24h;
(5) filter and washed screening to PH to less than 8, obtain houghite after drying.
Result: the houghite obtained is mainly calcium aluminium chlorine type houghite and calcium magnalium type houghite, is wherein mixed with a small amount of dephasign.
Embodiment 10
What the present embodiment provided utilizes blast furnace slag to prepare the method for zeolite compound, comprises the following steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, high temperature bath stirs, and makes the silicon part gel in blast furnace slag; Wherein blast furnace slag 10g, hydrochloric acid 60mL (3mol/L), bath temperature is 100 DEG C;
(2) filter, solution is divided into filtrate and gel two portions;
(3) after gel repetitive scrubbing, dry, grinding, obtains silica flour;
(4) in silica flour, add the sodium hydroxide solution violent stirring of 3mol/L, form uniform suspension liquid;
(5) to titration sodium aluminate solution in suspension liquid, and 0.5h is stirred;
(6) suspension liquid is moved into ageing 3h in Hydrothermal Synthesis still, temperature is 100 DEG C, and then filtration washing drying obtains product.
Result: obtain A-NaA zeolite.
Embodiment 11
The digestion time changed in embodiment 10 step (6) is 5h.
Result: obtain A-NaA zeolite.
Embodiment 12
The digestion time changed in embodiment 10 step (6) is 8h.
Result: obtain A-NaA zeolite.
Can be drawn by above-described embodiment and test result, utilize blast furnace slag to prepare houghite and zeolite, reach change and " give up " as precious object, what not only expand blast furnace slag utilizes scope, and improves the economic profit of blast furnace slag.
In above-described embodiment, embodiment 2,3,5,6,8,9,10,11,12 is preferred embodiment of the present invention.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (5)
1. utilize blast furnace slag to prepare a method for houghite and zeolite, it is characterized in that, comprise the steps:
(1) join in hydrochloric acid soln by the blast furnace slag of pulverizing, stir under boiling water bath, until the silicon part gel in blast furnace slag, be 50 ~ 60ml relative to the add-on of every gram of blast furnace slag hydrochloric acid, described concentration of hydrochloric acid is 3mol/L;
(2) filter, respectively filtrate and gel for subsequent use;
(3) in the filtrate of step (2) gained, dripping sodium hydroxide solution, is 9.5 ~ 13.5 to pH value, forms suspension liquid;
(4) suspension liquid will obtained in step (3), stirs 0.5 ~ 2h in 60 ~ 100 DEG C of constant water bath box, moves in Hydrothermal Synthesis still, ageing 12 ~ 24h at 60 ~ 100 DEG C;
(5) solution of step (4) ageing is filtered, and washed screening is to PH to less than 8, obtains houghite after drying;
(6) by after the gel repetitive scrubbing that obtains in step (2), dry, grinding, obtains silica flour;
(7) add sodium hydroxide solution violent stirring in the silica flour obtained to step (6), form uniform suspension liquid;
(8) in the suspension liquid obtained to step (7), titration is containing aluminum solutions, and stirs 0.5 ~ 1h;
(9) moved in Hydrothermal Synthesis still by the suspension liquid in step (8), bath temperature is 80 ~ 120 DEG C of ageing 3 ~ 8h, and then filtration washing drying obtains zeolite.
2. method according to claim 1, is characterized in that: in massfraction, described blast furnace slag comprises following compositions: SiO
2be 35 ~ 40%, CaO be 35 ~ 40%, MgO be 5 ~ 15%, Al
2o
3be 5 ~ 15%, surplus is trace ingredients.
3. method according to claim 1, is characterized in that: in step (3), and described concentration of sodium hydroxide solution is 2 ~ 4mol/L.
4. method according to claim 1, is characterized in that: in step (7), and described concentration of sodium hydroxide solution is 2 ~ 4mol/L.
5. method according to claim 1, is characterized in that: in step (8), and described is sodium aluminate solution or potassium aluminate solution containing aluminum solutions.
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| CN105671225A (en) * | 2016-01-22 | 2016-06-15 | 山东钢铁股份有限公司 | Method for comprehensively using blast furnace slag and converter slag |
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| CN106552662A (en) * | 2016-11-05 | 2017-04-05 | 上海大学 | The method that molecular sieve catalyst is prepared using smelting steel slag |
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| CN106552662A (en) * | 2016-11-05 | 2017-04-05 | 上海大学 | The method that molecular sieve catalyst is prepared using smelting steel slag |
| CN106552662B (en) * | 2016-11-05 | 2019-06-04 | 上海大学 | The method for preparing molecular sieve catalyst using steel slag is smelted |
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| CN109574084A (en) * | 2018-12-05 | 2019-04-05 | 上海宝田新型建材有限公司 | A kind of preparation method and applications of metallurgy base carbonate hydrotalcite |
| CN109574084B (en) * | 2018-12-05 | 2021-01-22 | 上海宝田新型建材有限公司 | Preparation method and application of metallurgical-base carbonate hydrotalcite |
| CN112174153A (en) * | 2020-09-11 | 2021-01-05 | 重庆大学 | Method for preparing A-type zeolite by utilizing titanium-containing blast furnace slag |
| CN113998706A (en) * | 2021-11-23 | 2022-02-01 | 重庆大学 | Method for preparing titanium-containing zeolite and co-producing titanium-containing hydrotalcite by using titanium-containing blast furnace slag |
| CN114408964A (en) * | 2022-01-22 | 2022-04-29 | 北京工业大学 | Method for preparing nano titanium-magnesium-aluminum-containing hydrotalcite from titanium-containing blast furnace slag |
| CN117401703A (en) * | 2023-10-11 | 2024-01-16 | 中国科学院过程工程研究所 | High-value utilization and synergistic carbon fixation method for blast furnace slag |
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