CN113800787A - Preparation method of high-activity calcium hydroxide - Google Patents
Preparation method of high-activity calcium hydroxide Download PDFInfo
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- CN113800787A CN113800787A CN202111162697.9A CN202111162697A CN113800787A CN 113800787 A CN113800787 A CN 113800787A CN 202111162697 A CN202111162697 A CN 202111162697A CN 113800787 A CN113800787 A CN 113800787A
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- Prior art keywords
- calcium hydroxide
- quicklime
- digestion
- additive
- calcium
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- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 title claims abstract description 75
- 239000000920 calcium hydroxide Substances 0.000 title claims abstract description 73
- 229910001861 calcium hydroxide Inorganic materials 0.000 title claims abstract description 73
- 230000000694 effects Effects 0.000 title abstract description 18
- 238000002360 preparation method Methods 0.000 title abstract description 7
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims abstract description 91
- 238000000034 method Methods 0.000 claims abstract description 57
- 239000000292 calcium oxide Substances 0.000 claims abstract description 47
- 235000012255 calcium oxide Nutrition 0.000 claims abstract description 47
- 239000000654 additive Substances 0.000 claims abstract description 36
- 230000000996 additive effect Effects 0.000 claims abstract description 29
- 230000008569 process Effects 0.000 claims abstract description 20
- 239000003546 flue gas Substances 0.000 claims abstract description 16
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000029087 digestion Effects 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 21
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 12
- 235000013539 calcium stearate Nutrition 0.000 claims description 12
- 239000008116 calcium stearate Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 11
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 9
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 9
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 9
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 5
- 229920000058 polyacrylate Polymers 0.000 claims description 5
- 238000011282 treatment Methods 0.000 claims description 5
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000035800 maturation Effects 0.000 claims 1
- 238000006477 desulfuration reaction Methods 0.000 abstract description 18
- 230000023556 desulfurization Effects 0.000 abstract description 18
- 238000000746 purification Methods 0.000 abstract description 8
- 239000004568 cement Substances 0.000 abstract description 4
- 239000002250 absorbent Substances 0.000 description 13
- 230000002745 absorbent Effects 0.000 description 13
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 12
- 229910052791 calcium Inorganic materials 0.000 description 12
- 239000011575 calcium Substances 0.000 description 12
- 239000008367 deionised water Substances 0.000 description 10
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 8
- 239000002002 slurry Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000011734 sodium Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 4
- 235000011941 Tilia x europaea Nutrition 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 239000010419 fine particle Substances 0.000 description 4
- 239000004571 lime Substances 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 235000019738 Limestone Nutrition 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 239000006028 limestone Substances 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 238000006703 hydration reaction Methods 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229920002121 Hydroxyl-terminated polybutadiene Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 241000208474 Protea Species 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- 230000010100 anticoagulation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- QTPSOVJLZXSTEB-UHFFFAOYSA-L calcium;dodecyl sulfate Chemical compound [Ca+2].CCCCCCCCCCCCOS([O-])(=O)=O.CCCCCCCCCCCCOS([O-])(=O)=O QTPSOVJLZXSTEB-UHFFFAOYSA-L 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- ANJPRQPHZGHVQB-UHFFFAOYSA-N hexyl isocyanate Chemical compound CCCCCCN=C=O ANJPRQPHZGHVQB-UHFFFAOYSA-N 0.000 description 1
- 238000007602 hot air drying Methods 0.000 description 1
- 239000004572 hydraulic lime Substances 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229940037627 magnesium lauryl sulfate Drugs 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- HBNDBUATLJAUQM-UHFFFAOYSA-L magnesium;dodecyl sulfate Chemical compound [Mg+2].CCCCCCCCCCCCOS([O-])(=O)=O.CCCCCCCCCCCCOS([O-])(=O)=O HBNDBUATLJAUQM-UHFFFAOYSA-L 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 229940080236 sodium cetyl sulfate Drugs 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- GGHPAKFFUZUEKL-UHFFFAOYSA-M sodium;hexadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCOS([O-])(=O)=O GGHPAKFFUZUEKL-UHFFFAOYSA-M 0.000 description 1
- NWZBFJYXRGSRGD-UHFFFAOYSA-M sodium;octadecyl sulfate Chemical compound [Na+].CCCCCCCCCCCCCCCCCCOS([O-])(=O)=O NWZBFJYXRGSRGD-UHFFFAOYSA-M 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2/00—Lime, magnesia or dolomite
- C04B2/02—Lime
- C04B2/04—Slaking
- C04B2/06—Slaking with addition of substances, e.g. hydrophobic agents ; Slaking in the presence of other compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/02—Oxides or hydroxides
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Biomedical Technology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geology (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Treating Waste Gases (AREA)
Abstract
The invention provides a preparation method of high-activity calcium hydroxide, which obtains the calcium hydroxide with high desulfurization efficiency by controlling the curing condition in the slaking process of quicklime. Furthermore, the method further improves the desulfurization efficiency of the prepared calcium hydroxide by means of reasonably using the additive, controlling the water-cement ratio, adjusting the dosage of the additive and the like. The invention also provides calcium hydroxide obtained by the method of the invention, and the application thereof in dry flue gas purification.
Description
Technical Field
The invention relates to a preparation method of high-activity calcium hydroxide, belonging to the technical field of gas pollution control.
Background
The dry flue gas purification technology is widely applied to the control of the emission of pollutants in industrial flue gas due to the advantages of simple operation, low maintenance and operation cost and the like. For SO2When acidic pollutants are in existence, spraying into a flue is generally adoptedRemoving the calcium-based or sodium-based absorbent. The sodium-based absorbent is usually sodium bicarbonate powder, has high reaction rate and high removal efficiency, but has relatively high material cost, easily causes certain economic pressure on enterprise production under the background of ultralow pollutant emission, and simultaneously, the generated desulphurization byproduct sodium sulfate can not be recycled at present, and secondary pollution is easily formed. Compared with a sodium-based absorbent, the calcium-based absorbent has lower cost, but has poorer pollutant removal effect. Because a compact calcium sulfate shell layer is formed on the outer layer of the large-particle calcium-based absorbent in the desulfurization process, the internal active components cannot be fully utilized, and the utilization rate of calcium is low. The calcium-based absorbent with high activity is developed to replace the existing high-cost sodium-based absorbent and the traditional calcium-based absorbent with low efficiency, and has important market value and application prospect.
In order to solve the above problems, the reactivity of the calcium-based absorbent and the utilization rate of calcium are generally enhanced by reducing the particle size of the absorbent and increasing the specific surface area and porosity of the absorbent in the prior art. For example, patent document 1 discloses a method for preparing high-activity nano calcium hydroxide, which uses a thermoreversible gel made of hydroxyl-terminated polybutadiene and n-hexyl isocyanate as a crystallization medium of calcium hydroxide, and adds stearate and urea at the same time to improve the crystal form of calcium hydroxide, provide the surface properties of nano calcium hydroxide, and the like. Patent document 2 discloses a process for preparing highly active anti-coagulation calcium hydroxide, which comprises crushing calcium oxide, performing multistage screening, performing multistage digestion, filtering, dehydrating, drying, screening and filtering to obtain calcium hydroxide. Patent document 3 discloses a method for preparing high-activity calcium hydroxide, which comprises mixing and digesting quicklime and additives such as diethylene glycol, sucrose or n-butanol to prepare calcium hydroxide slurry, aging, press-filtering, drying, and powdering to obtain calcium hydroxide slurry with a surface area of 15-60m2Calcium hydroxide particles per gram. Patent document 4 discloses an industrial preparation method of high-reactivity nano calcium hydroxide powder, which comprises the steps of treating and calcining limestone, pressure digestion of quicklime and final synthesis of nano calcium hydroxide to obtain nano calcium hydroxide powder with specific surface areaNot less than 50m2(ii) in terms of/g. Patent document 5 discloses a method for preparing nano calcium hydroxide powder for accelerating flue gas desulfurization, which includes subjecting hexagonal boron nitride, calcium chloride, aluminum-magnesium hydrotalcite, sodium hydroxide, an organic titanium catalyst and other substances to ultrasonic dissolution and mixing to prepare saturated clarified limewater, and subjecting the saturated clarified limewater to centrifugal washing and drying to obtain nano calcium hydroxide.
Cited documents:
patent document 1: CN111439768A
Patent document 2: CN108911535A
Patent document 3: CN112358205A
Patent document 4: CN112174179A
Patent document 5: CN112960684A
Disclosure of Invention
Problems to be solved by the invention
The methods disclosed in the prior art still do not meet the requirements. For example, the process of patent document 1 has a long production flow, a complicated process, and a high cost of chemical reagents used. The process of patent document 2 fails to cope with the particle size, surface area, and acidic gas, particularly SO, of the calcium hydroxide produced2The absorption properties of (a) are shown. In patent document 3, the amount of the additive is 4 to 6% of the mass of the quicklime, which may affect the removal performance of the acidic contaminants while increasing the cost. Patent document 4 has a complicated pretreatment process for raw quicklime, and has high requirements for quicklime activity and purity, resulting in a large early-stage investment. The additive used in patent document 5 has various types and harsh preparation conditions, which makes the control of the production process difficult and is not suitable for mass production.
Therefore, there is a need to develop a method for preparing high-activity calcium hydroxide, which can prepare high-activity calcium hydroxide at low cost, and the prepared calcium hydroxide can be used for dry flue gas purification.
Means for solving the problems
Aiming at the technical problems, the invention provides a preparation method of high-activity calcium hydroxide, which obtains the calcium hydroxide with high desulfurization efficiency by controlling the curing condition in the quicklime digestion process. Furthermore, the method further improves the desulfurization efficiency of the prepared calcium hydroxide by means of reasonably using the additive, controlling the water-cement ratio, adjusting the dosage of the additive and the like. The invention also provides calcium hydroxide obtained by the method of the invention, and the application thereof in dry flue gas purification.
Specifically, the present invention solves the technical problems to be solved by the present invention by the following means.
[1] A method for preparing calcium hydroxide, wherein the method comprises:
a digestion step: contacting quicklime with a digestion solution to carry out a digestion reaction to obtain a digestion material, wherein the digestion solution contains water;
curing step: standing the digested material at the temperature of 50-99 ℃; and
optionally a post-treatment step comprising one or more of dewatering, drying, crushing and sieving.
[2] The method according to [1], wherein the digestion solution further comprises an additive, and the additive is one or more selected from hydrogen peroxide, metal powder, alkyl sulfate, stearate, polyacrylate, triethanolamine, sodium tripolyphosphate and polyvinylpyrrolidone; preferably, the additive is one or more selected from hydrogen peroxide, aluminum powder, sodium dodecyl sulfate, calcium stearate, sodium polyacrylate and triethanolamine, sodium tripolyphosphate and polyvinylpyrrolidone.
[3] The method according to [1] or [2], wherein the ratio of the water to the quicklime is 5.5:1 to 0.5:1, preferably 5:1 to 1: 1.
[4] The method according to [2], wherein the additive in the digestion solution is 2% by mass or less, preferably 0.05% to 1% by mass of the quicklime.
[5] The method according to [1] or [2], wherein the aging step is performed for 0.5 to 3 hours, preferably 0.8 to 2 hours.
[6] The method according to [1] or [2], wherein the temperature of the aging step is 80 to 95 ℃.
[7] The method according to [1] or [2], wherein the digestion step is performed for 1 to 60 minutes, preferably 5 to 40 minutes.
[8] The method according to [1] or [2], wherein the particle size of the quicklime is 10 to 100mm, preferably 30 to 80 mm.
[9] Calcium hydroxide produced by the method according to any one of [1] to [8 ].
[10] Use of the calcium hydroxide according to [9] in dry flue gas cleaning.
ADVANTAGEOUS EFFECTS OF INVENTION
Compared with the traditional quicklime digestion technology, the method has simple operation flow and is easy to realize large-scale production, and the obtained calcium hydroxide has micron-sized ultrafine particle size and high reaction activity. The obtained calcium hydroxide powder is used for dry-method flue gas purification, and higher removal efficiency and higher calcium utilization rate than the traditional calcium-based absorbent can be obtained, so that the consumption of the absorbent can be reduced on the premise of meeting the existing flue gas purification standard.
Detailed Description
The present invention will be described in detail below. The technical features described below are explained based on typical embodiments and specific examples of the present invention, but the present invention is not limited to these embodiments and specific examples.
< terms and definitions >
In the present specification, "particle diameter" means the median diameter D of the particles described50It can be measured by a particle sizer.
In the present specification, the numerical range represented by "numerical value a to numerical value B" means a range including the end point numerical value A, B.
In the present specification, the numerical ranges indicated by "above" or "below" mean the numerical ranges including the numbers.
In the present specification, the meaning of "may" includes both the meaning of performing a certain process and the meaning of not performing a certain process.
As used herein, the use of "optionally" or "optional" means that certain materials, components, performance steps, application conditions, and the like are used or not used.
In the present specification, the unit names used are all international standard unit names, and the "%" used means weight or mass% content, if not specifically stated.
Reference throughout this specification to "a preferred embodiment," "an embodiment," and so forth, means that a particular element (e.g., feature, structure, property, and/or characteristic) described in connection with the embodiment is included in at least one embodiment described herein, and may or may not be present in other embodiments. In addition, it is to be understood that the described elements may be combined in any suitable manner in the various embodiments.
An object of the present invention is to provide a method for preparing calcium hydroxide, which comprises:
a digestion step: contacting quicklime with a digestion solution to carry out a digestion reaction to obtain a digestion material, wherein the digestion solution contains water;
curing step: standing the digested material at the temperature of 50-99 ℃; and
optionally a post-treatment step comprising one or more of dewatering, drying, crushing and sieving.
The individual steps of the process of the invention are described in detail below.
Digestion step
In the method of the present invention, calcium oxide in quicklime reacts with water in the digestion solution through a digestion step to generate calcium hydroxide. The quicklime used in the invention is blocky quicklime, and the particle size of the blocky quicklime is 10-100 mm, preferably 30-80 mm. The lump quicklime, particularly the lump quicklime having a particle size within the above range, locally generates a large amount of heat during a rapid hydration reaction with water, thereby causing rapid expansion and explosion of the lime lump, and thus generating fine particles.
The quicklime used in the present invention is not particularly limited, and it may be commercially available or prepared by a conventional method in the art. For example, it can be obtained by calcining natural rocks such as limestone, chalk, dolomitic limestone, etc., whose main component is calcium carbonate, at high temperature. Preferably, the calcium oxide content of the quicklime used in the present invention is above 90%, preferably above 95%.
The temperature of the digestion solution used in the digestion step is not particularly limited, and for example, the temperature of the digestion solution may be 20 to 80 ℃.
In one embodiment, the digestion step is performed for 1 to 60 minutes, if the digestion step is performed for less than 1 minute, the digestion process of the quicklime is not completely performed, and if the digestion step is performed for more than 60 minutes, the formed fine particles may be agglomerated to form larger particles. Preferably, the digestion step is performed for a time period of 5 to 40 minutes, more preferably 10 to 20 minutes.
In one embodiment, the digestion step is carried out under stirring conditions, so that the massive quicklime and the digestion solution can be more fully contacted and mixed by stirring, the digestion process is facilitated, and the agglomeration of small particles can be inhibited.
In one embodiment, the ratio of water to quicklime (hereinafter referred to as water-lime ratio) in the digestion solution is controlled within a range of 5.5:1 to 0.5:1, preferably 5:1 to 1:1, and more preferably 5:1 to 3: 1. If the water-cement ratio is too high, the reaction heat loss is easily caused and local heat accumulation cannot be quickly formed, so that the digestion process is too mild, and the generated fine particles are less; if the water-cement ratio is too low, the small water amount cannot meet the full-scale digestion of the quicklime, and especially when the local temperature is too high, a large amount of water is evaporated, so that the water is difficult to enter the inside of the quicklime to complete the digestion process, and the quicklime is not completely digested.
In a preferred embodiment, the digestion solution further comprises additives, the additives primarily serving to promote the formation and development of particle pores during digestion and to inhibit the agglomerate growth of small particles. The additive is one or more selected from hydrogen peroxide, metal powder, alkyl sulfate, stearate, polyacrylate, triethanolamine, sodium tripolyphosphate and polyvinylpyrrolidone. Wherein the metal powder may be, for example, aluminum powder or the like; the alkyl sulfate may be, for example, sodium lauryl sulfate, sodium cetyl sulfate, sodium stearyl sulfate, calcium lauryl sulfate, magnesium lauryl sulfate, etc.; the stearate may be, for example, calcium stearate, magnesium stearate, zinc stearate, calcium stearate, etc.; the polyacrylate salt can be, for example, sodium polyacrylate, calcium polyacrylate, and the like.
In a further preferred embodiment, the additive is one or more selected from the group consisting of hydrogen peroxide, aluminum powder, sodium lauryl sulfate, calcium stearate, sodium polyacrylate and triethanolamine, sodium tripolyphosphate, and polyvinylpyrrolidone.
In a further preferred embodiment, the additive is one or more selected from the group consisting of hydrogen peroxide, sodium lauryl sulfate, calcium stearate, triethanolamine, and sodium tripolyphosphate. In a more preferred embodiment, the additive is hydrogen peroxide and calcium stearate, triethanolamine, calcium stearate and sodium lauryl sulfate, or sodium tripolyphosphate.
The amount of the additive is 2% or less, preferably 1% or less, and more preferably 0.5% or less by mass of the raw lime material. Excessive additive usage will affect the pore development of the calcium hydroxide particles and also cause an increase in the production cost. The amount of the additive is 0.01% or more, preferably 0.03% or more, and more preferably 0.05% or more, by mass of the raw material of quicklime, from the viewpoint of sufficiently exerting the effect of the additive.
Aging step
In the method, the quicklime is sufficiently digested and decomposed through the slaking step, and the calcium hydroxide with high activity is generated.
The present inventors have found that the calcium hydroxide product obtained by slaking a lime slurry, i.e. a slaked material, under standing conditions is more active than slaking under stirring conditions. And the slaking at a higher temperature is very critical to the hydration reaction process, too high temperature can cause a large amount of water vapor to be generated, the water vapor is not beneficial to the formation of calcium hydroxide pores in the slaking stage, and too low temperature can cause the unsmoked quicklime in the lime to be slowly slaked in the slaking process to form larger calcium hydroxide particles. The present invention has been made on the basis of such a finding.
In a specific embodiment, in the method of the present invention, the aging step is performed by allowing the digested material to stand at a temperature of 50 to 99 ℃ for aging. In a preferred embodiment, the curing temperature is 80 to 95 ℃.
The curing time may be 0.5 to 3 hours, preferably 0.8 to 2 hours. Too short a slaking time may result in incomplete slaking of the quicklime and a reduction in the yield and quality of the calcium hydroxide, while too long a slaking time may result in agglomeration of the formed fine particles to form larger particles.
Other steps
The process of the present invention optionally further comprises a step of post-treating the calcium hydroxide slurry obtained in the slaking step, said post-treatment step comprising dewatering, drying and optionally further post-treatments, such as crushing, sieving steps and the like.
These steps may be performed in a manner conventional in the art. For example, the dehydration step may be performed by using a dehydration device such as a filter press, a centrifuge, or a suction filter, and the calcium hydroxide slurry obtained in the aging step is preliminarily dehydrated to reduce the water content of the slurry to 30% or less. The drying step can be carried out by adopting equipment such as a hot air drying oven, rotary drying, spray drying and the like, and the calcium hydroxide slurry subjected to preliminary dehydration is dried, and the water content of the calcium hydroxide obtained after drying is less than 5%. Optionally, the dried calcium hydroxide may be fed into a pulverizing device such as a ball mill, a Raymond mill, a micronizer, or a jet mill for final pulverization, and the particle size of the calcium hydroxide may be sieved. The screening step can be carried out by adopting a screen with 100-500 meshes.
By the method of the present invention, calcium hydroxide having high desulfurization efficiency can be obtained, which has a breakthrough time of 40min or more, preferably 60min or more, in the desulfurization test. In embodiments where additives are used, the breakthrough time of the calcium hydroxide obtained by the process of the invention in desulfurization tests may be up to 65min or more, and in some embodiments up to 70min or more, and in particularly preferred embodiments up to 90min or more.
The invention also relates to the calcium hydroxide prepared by the method of the invention and the application of the calcium hydroxide in dry-method flue gas purification.
The present invention will be further described below by way of specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the description of the present invention, and such equivalents also fall within the scope of the invention.
Examples
Example 1: 10g of a lump quicklime sample having a particle size of 40mm was weighed, placed in a beaker containing 50mL of normal temperature deionized water, subjected to a digestion reaction for 10 minutes under stirring, and then transferred to a constant temperature water bath of 90 ℃ for standing and aging for 1 hour. And (3) carrying out suction filtration and washing on the cured sample, placing the sample in an air drying oven to be dried at 105 ℃, and then grinding and screening the sample to obtain a calcium hydroxide sample with the particle size of more than 200 meshes.
Comparative example 1: a calcium hydroxide sample was prepared in the same manner as in example 1, except that the aging step was performed at room temperature.
Example 2: a calcium hydroxide sample was prepared in the same manner as in example 1, except that deionized water was used in an amount of 10mL, i.e., a water-to-ash ratio of 1.
Example 3: except that 0.05 wt% of H based on the mass of quicklime is added to deionized water2O2And 0.05 wt% of calcium stearate as an additive, a calcium hydroxide sample was prepared in the same manner as in example 1.
Example 4: a calcium hydroxide sample was prepared in the same manner as in example 1, except that triethanolamine was added as an additive in an amount of 0.1 wt% based on the mass of quicklime to deionized water.
Example 5: a calcium hydroxide sample was prepared in the same manner as in example 1, except that 0.05 wt% of triethanolamine and 0.05 wt% of calcium stearate, based on the mass of quicklime, were added as additives to deionized water.
Example 6: a calcium hydroxide sample was prepared in the same manner as in example 1, except that 0.1 wt% of aluminum powder and 0.1 wt% of calcium stearate based on the mass of quicklime were added as additives to deionized water.
Example 7: a calcium hydroxide sample was prepared in the same manner as in example 1, except that 0.1 wt% of sodium lauryl sulfate and 0.1 wt% of calcium stearate based on the mass of quicklime were added as additives to deionized water.
Example 8: a calcium hydroxide sample was prepared in the same manner as in example 1, except that 0.1 wt% of sodium polypropylene, based on the mass of quicklime, was added as an additive to deionized water.
Example 9: a calcium hydroxide sample was prepared in the same manner as in example 1, except that 1 wt% of sodium tripolyphosphate was added as an additive to deionized water based on the mass of quicklime.
Example 10: a calcium hydroxide sample was prepared in the same manner as in example 1, except that 1 wt% of polyvinylpyrrolidone based on the mass of quick lime was added as an additive to deionized water.
Desulfurization Performance test
The calcium hydroxide powders obtained in examples 1 to 10 and comparative example 1 were each subjected to a desulfurization performance test using a fixed bed reactor. The inner diameter of the adopted fixed bed reactor is 10mm, the reaction temperature is controlled to be 300 ℃, and the simulated flue gas is SO2、O2And N2In which SO is2At a concentration of 500ppmv, O2The concentration is 10 percent, the rest is nitrogen component, and the flow rate of flue gas is 500 mL/min.
For all samples, the desulfurization performance test was performed using a sample size of 150mg of available calcium content to ensure comparability between different samples. Import and export SO2The concentration is determined by infrared spectroscopyAssay by analyzer (Protea).
The desulfurization efficiency of the sample was calculated according to the following formula:
in the formula: rho1Is an inlet SO2Flue gas concentration in mg/m3Denotes ρ2Is an outlet SO2Flue gas concentration in mg/m3As shown, eta SO2 is the desulfurization efficiency.
In the desulfurization test, for each sample, the SO was recorded2The time elapsed for the removal efficiency to drop to 30%, defined as the breakthrough time of the reaction, the longer the breakthrough time the better the desulfurization performance of the calcium hydroxide. The results are shown in Table 1.
TABLE 1
Wherein the English abbreviation means as follows:
SDS (sodium dodecyl sulfate): sodium dodecyl sulfate
PVP: polyvinylpyrrolidone
As can be seen from Table 1, the penetration time of the calcium hydroxide sample obtained in example 1 which was aged by standing at 90 ℃ was significantly higher than that of comparative example 1 which was aged by standing at room temperature, indicating that the calcium hydroxide having a better desulfurization effect can be obtained by standing at a higher temperature in the present invention.
Further, examples 2 to 10 further improved the desulfurization efficiency of calcium hydroxide by using the additive, as compared with example 1 in which no additive was used.
Industrial applicability
The method can be widely used for preparing high-activity sodium hydroxide, and the obtained calcium hydroxide can be used as a desulfurizer to be widely used in dry flue gas purification.
Claims (10)
1. A method for preparing calcium hydroxide, wherein the method comprises:
a digestion step: contacting quicklime with a digestion solution to carry out a digestion reaction to obtain a digestion material, wherein the digestion solution contains water;
curing step: standing the digested material at the temperature of 50-99 ℃; and
optionally a post-treatment step comprising one or more of dewatering, drying, crushing and sieving.
2. The method of claim 1, wherein the digestion solution further comprises an additive, wherein the additive is one or more selected from hydrogen peroxide, metal powder, alkyl sulfate, stearate, polyacrylate, triethanolamine, sodium tripolyphosphate, and polyvinylpyrrolidone; preferably, the additive is one or more selected from hydrogen peroxide, aluminum powder, sodium dodecyl sulfate, calcium stearate, sodium polyacrylate and triethanolamine, sodium tripolyphosphate and polyvinylpyrrolidone.
3. A method according to claim 1 or 2, wherein the ratio of water to quicklime is 5.5:1 to 0.5:1, preferably 5:1 to 1: 1.
4. A method according to claim 2, wherein the mass of the additive in the digestion solution is 2% or less, preferably 0.05-1% of the mass of the quicklime.
5. A process according to claim 1 or 2, wherein the maturation step is carried out for a period of 0.5 to 3 hours, preferably 0.8 to 2 hours.
6. The method according to claim 1 or 2, wherein the temperature of the aging step is 80 to 95 ℃.
7. A method according to claim 1 or 2, wherein the digestion step is carried out for a period of 1 to 60 minutes, preferably 5 to 40 minutes.
8. A method according to claim 1 or 2, wherein the quicklime has a particle size of 10 to 100mm, preferably 30 to 80 mm.
9. Calcium hydroxide produced by the process according to any one of claims 1 to 8.
10. Use of calcium hydroxide according to claim 9 in dry flue gas cleaning.
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