CN117446814A - Method for preparing calcium silicate by using gas slag - Google Patents
Method for preparing calcium silicate by using gas slag Download PDFInfo
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- CN117446814A CN117446814A CN202311764692.2A CN202311764692A CN117446814A CN 117446814 A CN117446814 A CN 117446814A CN 202311764692 A CN202311764692 A CN 202311764692A CN 117446814 A CN117446814 A CN 117446814A
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- calcium silicate
- slag
- gas slag
- roasting
- gas
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- 239000002893 slag Substances 0.000 title claims abstract description 119
- 239000000378 calcium silicate Substances 0.000 title claims abstract description 53
- 229910052918 calcium silicate Inorganic materials 0.000 title claims abstract description 53
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000000034 method Methods 0.000 title claims abstract description 39
- 238000002156 mixing Methods 0.000 claims abstract description 24
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical group [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002244 precipitate Substances 0.000 claims abstract description 15
- 230000004913 activation Effects 0.000 claims abstract description 13
- 238000000967 suction filtration Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 9
- 238000004090 dissolution Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000000243 solution Substances 0.000 claims description 29
- 239000003034 coal gas Substances 0.000 claims description 19
- 239000007790 solid phase Substances 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 17
- 238000002309 gasification Methods 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000003245 coal Substances 0.000 claims description 12
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 18
- 238000006243 chemical reaction Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 13
- 239000000377 silicon dioxide Substances 0.000 abstract description 9
- 239000007787 solid Substances 0.000 abstract description 9
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 7
- 239000000706 filtrate Substances 0.000 abstract description 7
- 239000011575 calcium Substances 0.000 abstract description 6
- 229910052791 calcium Inorganic materials 0.000 abstract description 6
- 238000001914 filtration Methods 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 4
- 239000011550 stock solution Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 8
- -1 iron ions Chemical class 0.000 description 8
- 239000011734 sodium Substances 0.000 description 8
- 239000002245 particle Substances 0.000 description 7
- 239000004115 Sodium Silicate Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 229910052911 sodium silicate Inorganic materials 0.000 description 6
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052742 iron Inorganic materials 0.000 description 5
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 4
- 238000005265 energy consumption Methods 0.000 description 4
- 229910001425 magnesium ion Inorganic materials 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- 229910001424 calcium ion Inorganic materials 0.000 description 3
- 239000002910 solid waste Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910004762 CaSiO Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229910001415 sodium ion Inorganic materials 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229960004887 ferric hydroxide Drugs 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000008236 heating water Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 1
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 229910001437 manganese ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003376 silicon Chemical class 0.000 description 1
- XJKVPKYVPCWHFO-UHFFFAOYSA-N silicon;hydrate Chemical compound O.[Si] XJKVPKYVPCWHFO-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/24—Alkaline-earth metal silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to the technical field of comprehensive utilization of gas slag, in particular to a method for preparing calcium silicate by using gas slag; mixing, crushing, grinding and other pretreatment of the gas slag, roasting the pretreated gas slag, carrying out acid dissolution on the roasted gas slag, heating and stirring in a water bath, carrying out suction filtration after full reaction, obtaining a filtrate rich in calcium elements after filtration, mixing the filtrate with a stable solid of a silicon dioxide phase, adjusting the pH of the filtrate, removing other metal impurities, uniformly mixing the solid of the silicon dioxide phase with sodium carbonate, carrying out activation roasting, dissolving activated silicon element in water in a water glass form, adding water glass into a stock solution rich in calcium elements, and obtaining a calcium silicate precipitate, and filtering, washing and drying the calcium silicate precipitate to obtain a calcium silicate solid with higher purity; extracting valuable elements such as Si, ca and the like from the gas slag through a set of process flow to prepare the calcium silicate.
Description
Technical Field
The invention relates to the technical field of comprehensive utilization of gas slag, in particular to a method for preparing calcium silicate by using gas slag.
Background
The coal gasification slag is a byproduct generated in the coal gasification process; coal gasification is a process of converting solid coal into combustible gas, which needs to be performed at high temperature and high pressure; in this process, the coal is heated to an elevated temperature to cause a thermochemical reaction, and some solid waste including cinder, ash, and char is produced during gasification; these solid wastes are commonly referred to as gas-related slags.
The coal gasification residue comprises coarse residue and fine residue, the residue components are related to the ash content, composition, gasification process and the like of the gasification raw material coal, and the contents of Si, fe, al, ca and the like in the coarse residue and the fine residue are more.
Disclosure of Invention
The invention aims to provide a method for preparing calcium silicate by utilizing gas slag, which is used for extracting valuable elements such as Si, ca and the like from the gas slag through a set of process flows to prepare the calcium silicate.
The technical scheme adopted by the invention is as follows: a method for preparing calcium silicate by using gas slag,
s1: mixing, crushing and grinding the coarse coal gas slag and the fine coal gas slag;
s2: roasting the gas slag after grinding of the S1;
s3: adding hydrochloric acid into the gasified slag after roasting in the step S2 for dissolution, and stirring in a hot water bath; suction filtration is carried out to obtain a first solution and a first solid phase;
s4: adding an alkaline solution to adjust the pH value of the first solution to 5-6, and then carrying out suction filtration to obtain a second solution and a second solid phase;
s5: washing the first solid phase in the step S3, uniformly mixing with sodium carbonate, and performing activation roasting;
s6: dissolving out the silicon element heated water activated in the step S5 in a water glass mode;
s7: adding the water glass obtained in the step S6 into the second solution to obtain calcium silicate precipitate;
s8: and (3) after the calcium silicate precipitates are filtered, washing and drying are carried out, and a high-purity calcium silicate product is obtained.
In the step S1, the mixing ratio of the coarse gas-chemical slag and the fine gas-chemical slag is 5:1-1.5.
Further, in step S2, the roasting temperature is 730 ℃, the roasting time is 40mins, and the heating rate is 15 ℃/min.
Further, in step S3, the mass fraction of hydrochloric acid was 31%, and the mixture was stirred for 10 minutes, and the temperature of the hot water bath was 80 ℃.
Further, in step S4, the alkaline solution used is a sodium hydroxide or potassium hydroxide solution.
Further, in step S4, the pH of the first solution is adjusted to 6.
Further, in step S5, the first solid phase is uniformly mixed with sodium carbonate 1:1, and uniformly mixing the components.
Further, in step S5, the activation baking is performed at 830℃for 70mins.
Further, in step S8, the drying temperature was 80℃and the drying time was 2 hours.
The beneficial effects achieved by the invention are as follows:
1. the invention relates to a method for preparing calcium silicate by using gas slag, which comprises the steps of firstly carrying out pretreatment such as mixing, crushing, grinding and the like on the gas slag, adopting a mechanical method to reduce the particle size of ore and increase the surface area, then roasting the pretreated gas slag, and utilizing residual carbon of a fine slag part to provide heat so as to enable coarse slag of a glass phase to be loose and porous; the gas slag after roasting is subjected to strong acid dissolution and water bath heating and stirring, so as to completely dissolve the metal oxide intoFiltering after the metal ions fully react, obtaining filtrate rich in calcium element after filtering, mixing the filtrate with solid of stable silicon dioxide phase, and adjusting pH of the filtrate to enable metal impurity ions such as iron ions, aluminum ions and the like in the filtrate to be precipitated as hydroxide, so as to remove other metal impurities; uniformly mixing the solid of the silicon dioxide phase with sodium carbonate, and performing activation roasting to perform chemical reaction: na (Na) 2 CO 3 + SiO 2 == Na 2 SiO 3 + CO 2 ∈ aiming at converting stable silica into active sodium silicate, dissolving activated silicon element heating water in the form of sodium silicate, adding the sodium silicate into a stock solution rich in calcium element, and carrying out chemical reaction: na (Na) 2 SiO 3 +CaCl 2 ==CaSiO 3 And ∈+2NaCl to obtain calcium silicate precipitate, and filtering, water washing and drying the calcium silicate precipitate to obtain high purity calcium silicate solid. The calcium silicate prepared by the method has higher purity, smaller granularity, capability of just reacting with calcium silicate, green and no pollution.
2. The method for preparing the calcium silicate by using the gas slag adopts the main modes of separating calcium and silicon by strong acid, purifying, activating and roasting respectively, and utilizes the characteristics of the gas slag of the ratio of calcium to silicon of 1, thereby solving the problems of taking the gas slag as industrial solid waste, causing environmental pollution, occupying a large amount of land for stacking, realizing high-value utilization and the like, and avoiding the problems of low purity, easy caking and adhesion and the like of the traditional slag preparation of the calcium silicate. The method for preparing the calcium silicate has the advantages of high purity, small granularity, environment friendliness, no pollution, simple process device, low investment, low energy consumption, quick reaction, easy control, easy industrialization, continuous production and the like.
Drawings
FIG. 1 is a graph of the ratios of the components of the coarse and fine gas-converted slag of the present invention.
Fig. 2 is a process flow diagram of the present invention.
Fig. 3 is an SEM image of the fine slag of the present invention.
FIG. 4 is an SEM-EDS of elemental calcium, silicon, oxygen of the present invention.
FIG. 5 is a graph of the particle size of calcium silicate of the present invention.
Fig. 6 is a diagram of a calcium silicate product of the present invention.
FIG. 7 is a schematic view showing precipitation of elemental silicon water glass according to the present invention.
FIG. 8 is a schematic diagram of the coarse slag roasting of the gas-converted slag of the present invention.
FIG. 9 is a schematic diagram of the fine slag roasting of the gas-converted slag of the present invention.
FIG. 10 is a schematic diagram of the mixed roasting of coarse and fine gas-converted slag of the present invention.
Detailed Description
In order to facilitate understanding of the invention by those skilled in the art, a specific embodiment of the invention is described below with reference to the accompanying drawings.
First, an application scenario of the present application is described: generally, the production amount of the gas slag coarse slag accounts for about 80 percent of the total emission amount of the gasification slag, the carbon residue content is lower, generally 5-30 percent, and the grain size of the gas slag coarse slag is 16-4 meshes; the coal gas slag is about 20% of the total discharge amount of the gasified slag, the gasification residence time of the coal gas slag in the gasifier is short, the mass fraction of carbon residue is high, the mass fraction is about 30% -50%, and the particle size of the coal gas slag is smaller than 200 meshes; the sources and the states of gasified slag generated by different coal gasification processes are different; the ratios of the components (after decarbonizing) of the coarse coal gasification slag and the fine coal gasification slag adopted in the test are shown in figure 1.
As shown in fig. 2, the present invention provides a method for preparing calcium silicate by using gas slag, comprising the following steps:
s1: mixing, crushing and grinding the coarse coal gas slag and the fine coal gas slag;
specifically, the coarse coal gas slag is crushed by a crusher and then ground by a mill (250-4000 microns), and the particle size of the ground coarse coal gas slag is 1000-70 meshes, preferably 300 meshes; the particle size of the coarse slag is reduced by adopting a physical method, and the particle size of the coarse slag is still larger than that of the fine slag; the mixing ratio of the coarse coal gas slag to the fine coal gas slag is 5:1-1.5; preferably 5:1.
S2: roasting the gas slag after grinding of the S1;
specifically, a trolley furnace is adopted for roasting, the roasting temperature is 550-750 ℃, the roasting time is 20-60mins, and the heating rate is 10-20 ℃/min; and removing all residual carbon in the coarse slag and the fine slag through roasting treatment.
The reason why the coarse slag and the fine slag are used together as raw materials in the present application is as follows:
firstly, the components contained in the coarse coal gas slag and the fine coal gas slag are the same, and valuable elements can be extracted through a set of processes;
and secondly, compared with the method that coarse slag is independently used as a raw material, the method has the advantages that the roasting temperature can be greatly reduced and the energy consumption can be reduced by doping fine slag. The reason for this is as follows: first, as shown in FIG. 3, which is an electron microscopic image of fine slag, carbon in the fine slag exists in each part in a flocculent form; secondly, the carbon content in the fine slag is about 30-50%, and the carbon content of the coarse slag is high; in the application, the coarse slag and the fine slag are mixed, crushed and ground to ensure that the fine slag is uniformly distributed in the reaction materials; in the roasting process, all parts of carbon uniformly distributed in the reaction materials are combusted at the same time to release heat, and the heat generated by carbon combustion directly acts on the surface and the inside of gasified slag, so that the temperature provided by roasting equipment is greatly reduced, and the aim of reducing energy consumption is fulfilled; it was estimated that complete combustion of 1kg carbon-containing slag can generate about 32825.56KJ of heat; the roasting temperature of the raw materials of the coarse slag is required to reach 750-850 ℃ independently, and after the fine slag is doped, the roasting temperature is reduced to 550-750 ℃, so that the energy consumption is reduced; in addition, through tests, compared with the single reaction speed of the coarse slag, the mixed reaction of the coarse slag and the fine slag is faster, so that the roasting time is shortened;
s3: adding hydrochloric acid into the gasified slag after roasting in the step S2 for dissolution, and stirring in a hot water bath; then carrying out suction filtration to obtain a first solution and a first solid phase;
specifically, adding hydrochloric acid with the mass fraction of 31% until the precipitate is no longer dissolved; the temperature of the hot water bath is 80-90 ℃, the heating temperature of the water bath is adjustable, the heating is stable, the dissolution speed can be accelerated, and the stirring is carried out for 10 minutes; the suction filtration can be carried out through a buchner funnel, a suction filtration bottle, a circulating vacuum pump and the like for solid-liquid separation;
the reaction occurring in step S3 is as follows: mnO+2HCl→MnCl 2 +H 2 O
MgO+2HCl→MgCl 2 +H 2 O
Fe 2 O 3 +6HCl→2FeCl 3 +3H 2 O
The manganese element and the magnesium element which are mainly separated are completely dissolved in the solution in the form of manganese ions and magnesium ions; alO (aluminum oxide) 3 、CaO、Fe 2 O 3 Respectively aluminum chloride, calcium chloride, ferric chloride and the like in the first solution;
the pH value of the detected first solution is less than 1, and the first solution contains valuable metal ion solutions such as magnesium ions, aluminum ions, iron ions, calcium ions and the like; the first solid phase is SiO 2。
S4: adding an alkaline solution to adjust the pH value of the first solution to 5-6, and then carrying out suction filtration to obtain a second solution and a second solid phase;
further, the alkaline solution used in step S4 is sodium hydroxide or potassium hydroxide solution, preferably sodium hydroxide solution, preferably pH 6; at this time, iron and aluminum are completely precipitated;
the reaction occurring in step S4 is as follows: fe (Fe) 3+ +Na0H→Fe(0H) 3 ↓+Na +
Al 3+ +Na0H→Al(0H) 3 ↓+Na +
So that iron ions generate ferric hydroxide precipitates and aluminum ions generate aluminum hydroxide precipitates; sodium ions, calcium ions and magnesium ions are still in the solution in the form of ions;
through detection, the second solid phase contains impurities such as iron, aluminum and the like; the main components in the second solution are calcium ions, sodium ions and magnesium ions;
s5: washing the first solid phase in the step S3, uniformly mixing with sodium carbonate, and performing activation roasting;
specifically, the first solid phase is silica, and the mixing ratio of the silica to sodium carbonate is 1 (0.8-1.2), preferably 1:1; uniformly mixing by a stirrer, roasting by a trolley furnace, wherein the activation roasting temperature is 750-950 ℃ and the time is 60-120mins, preferably 70mins;
the reaction occurring in step S5 is as follows: na (Na) 2 CO 3 + SiO 2 ==Na 2 SiO 3 + CO 2 ↑
Uniformly mixing the solid of the silica phase with sodium carbonate, and performing activation roasting to convert the stable silica into active sodium silicate; silicate ions are provided for subsequent reactions.
The method comprises the steps of roasting coarse coal gas slag and fine coal gas slag, and dissolving acid to form a first solid phase; uniformly mixing the first solid phase with sodium carbonate, and performing activation treatment; the reason that the process is carried out according to the process sequence of roasting, acid dissolution and activation is as follows: in order to separate the metal component from the silicon component, a calcium-rich solution and a sodium silicate solution are obtained respectively, and then calcium silicate is synthesized, the purity of the calcium silicate obtained by the sequence is higher, and the adverse effects of reduced sodium silicate yield, high impurity content of the calcium solution and the like are caused after the sequence is adjusted.
S6: dissolving out the silicon element heated water activated in the step S5 in a water glass (sodium silicate) form;
specifically, the temperature of the hot water is 80-90 ℃, preferably 90 ℃, and the water glass is shown in the figure;
s7: adding the water glass obtained in the step S6 into the second solution to obtain calcium silicate precipitate;
specifically, the reaction occurring in step S7 is as follows: na (Na) 2 SiO 3 +CaCl 2 ==CaSiO 3 ↓+2NaCl；
S8: filtering the calcium silicate precipitate, washing and drying to obtain a high-purity calcium silicate product;
specifically, suction filtration is adopted for filtration, and the vacuum degree is 0.05-0.1MPa; washing by distilled water, and heating the air blowing box at the drying temperature of 80 ℃ for 2 hours;
the purity of the detected calcium silicate solids was: 95.13%
As shown in SEM-EDS diagram of fig. 4, the mass ratio and atomic ratio of the sample are shown in table 1 below, which corresponds to the chemical structure of calcium silicate;
the traditional slag preparation uses clay, which is easy to cause caking and adhesion, and the calcium silicate has low purity and is easy to agglomerate and adhere; the purity of the calcium silicate prepared by the method is higher, as shown in figure 5, and the granularity of the prepared calcium silicate is smaller than 2.5; meanwhile, the problems of low purity, easy caking and adhesion and the like in the traditional slag preparation of calcium silicate are avoided; as shown in fig. 6, the calcium silicate prepared by the method is not easy to be adhered by a water preparation method.
Example 1
The invention discloses a method for preparing calcium silicate by using gas slag, which comprises the following steps:
s1: mixing, crushing and grinding the coarse coal gas slag and the fine coal gas slag in a ratio of 5:1, wherein the grinding particle size is 300 meshes;
s2: roasting the gas slag after grinding of the S1; the roasting temperature is 730 ℃, the roasting time is 40mins, and the heating rate is 15 ℃/min;
s3: adding hydrochloric acid into the gasified slag after the activation in the step S2 for dissolution, wherein the mass fraction of the hydrochloric acid is 31%; stirring for 60min at 80deg.C in hot water bath until the precipitate is no longer dissolved; then carrying out suction filtration to obtain a first solution and a first solid phase;
s4, adding sodium hydroxide to adjust the pH value of the first solution to 6, and then carrying out suction filtration to obtain a second solution and a second solid phase;
s5, washing the first solid phase in the step S3, and mixing with sodium carbonate in a ratio of 1:1, and carrying out activation roasting by a trolley furnace, wherein the roasting temperature is 830 ℃ and the time is 70mins;
s6, adding hot water at 90 ℃ into the silicon element activated in the step S5 to dissolve out in a water glass form, as shown in figure 7;
s7, adding the water glass obtained in the step S6 into the second solution to obtain calcium silicate precipitate;
s8, carrying out suction filtration on calcium silicate by the vacuum degree of 0.1MPa; and then washing by distilled water, and drying by an electrothermal blowing box at the drying temperature of 80 ℃ for 2 hours.
Experiment 1 researches the influence on activated gasification slag by adding coarse slag of gas gasification slag and fine slag of gas gasification slag separately and mixing the coarse slag and the fine slag.
Comparative example 1
In this comparative example, the same amount of crude gas-converted slag as in example was added alone, and the other conditions were the same as in example.
Comparative example 2
In this comparative example, the same amount of the fine slag of the gas slag as in example was added alone, and the crushing and grinding were not performed, and the other conditions were the same as in example.
Experimental results
As shown in Table 2 below, examples of the present application and comparative examples 1 and 2 are shown, activated gasified slag was obtained and analyzed
The embodiments of the present invention described above do not limit the scope of the present invention. Any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should be included in the scope of the present invention as set forth in the appended claims.
Claims (9)
1. A method for preparing calcium silicate by using gas slag is characterized in that:
s1: mixing, crushing and grinding the coarse coal gas slag and the fine coal gas slag;
s2: roasting the gas slag after grinding of the S1;
s3: adding hydrochloric acid into the gasified slag after roasting in the step S2 for dissolution, and stirring in a hot water bath; suction filtration is carried out to obtain a first solution and a first solid phase;
s4: adding an alkaline solution to adjust the pH value of the first solution to 5-6, and then carrying out suction filtration to obtain a second solution and a second solid phase;
s5: washing the first solid phase in the step S3, uniformly mixing with sodium carbonate, and performing activation roasting;
s6: dissolving out the silicon element heated water activated in the step S5 in a water glass mode;
s7: adding the water glass obtained in the step S6 into the second solution to obtain calcium silicate precipitate;
s8: and (3) after the calcium silicate precipitates are filtered, washing and drying are carried out, and a high-purity calcium silicate product is obtained.
2. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in the step S1, the mixing ratio of the coarse coal gasification slag to the fine coal gasification slag is 5:1-1.5.
3. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in the step S2, the roasting temperature is 730 ℃, the roasting time is 40mins, and the heating rate is 15 ℃/min.
4. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in the step S3, the mass fraction of hydrochloric acid is 31%, and the mixture is stirred for 10 minutes, and the temperature of the hot water bath is 80 ℃.
5. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in step S4, the alkaline solution used is sodium hydroxide or potassium hydroxide solution.
6. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in step S4, the pH of the first solution is adjusted to 6.
7. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in step S5, the first solid phase is uniformly mixed with sodium carbonate 1:1, and uniformly mixing the components.
8. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in the step S5, the activation roasting is performed, the roasting temperature is 830 ℃, and the time is 70mins.
9. The method for preparing calcium silicate by using gas slag according to claim 1, wherein: in step S8, the drying temperature is 80℃and the drying time is 2 hours.
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