CN114210192A - Process for preparing high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag - Google Patents

Process for preparing high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag Download PDF

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CN114210192A
CN114210192A CN202111558750.7A CN202111558750A CN114210192A CN 114210192 A CN114210192 A CN 114210192A CN 202111558750 A CN202111558750 A CN 202111558750A CN 114210192 A CN114210192 A CN 114210192A
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slag
clear liquid
calcium oxide
carbide slag
solution
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丁顶
王明建
欧明乐
赵安亮
张源
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Anhui Hwasu Corp
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    • 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
    • B01D53/77—Liquid phase processes
    • B01D53/78—Liquid phase processes with gas-liquid contact
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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
    • B01D53/46—Removing components of defined structure
    • B01D53/48—Sulfur 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
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
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    • B82—NANOTECHNOLOGY
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    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
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    • 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
    • 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
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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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Abstract

The invention discloses a process for preparing a high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag, which comprises the following steps: 1) putting the carbide slag into a hydrocyclone to obtain clear liquid I and slurry I; 2) mixing the slurry I with hydrochloric acid, stirring and pressingFiltering to obtain insoluble substances and turbid liquid; 3) adding NH into the turbid liquid3·H2O, centrifuging after ball milling to obtain slurry II and clear liquid II; 4) adding NH into clear liquid II4HCO3Stirring and filtering to obtain a precipitate and a filtrate, and drying and decomposing the precipitate to obtain active calcium oxide; 5) adding a flocculating agent into the filtrate, and aging to obtain floccules and clear liquid III; 6) production of NH from clear liquor III4HCO3The solution is returned for use. The method provided by the invention can be used for more finely screening and treating more than 98% of the components of the carbide slag, so that finally, no waste slag is generated, and a systematic platform is provided for the consumption of all the components; the invention realizes the basic recycling of ammonia and water and has lower cost.

Description

Process for preparing high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag
Technical Field
The invention relates to the technical field of recycling of carbide slag, in particular to a process for preparing a high-efficiency desulfurizer and a byproduct of active calcium oxide by using carbide slag.
Background
Acetylene is one of important raw materials of PVC (polyvinyl chloride) by a calcium carbide method, and is usually generated by adding water (wet method) into calcium carbide serving as a raw material and simultaneously generating a certain amount of industrial waste liquid, commonly called as calcium carbide slag slurry. The carbide slag contains carbide slag and percolate with certain water content, and also contains toxic and harmful substances such as sulfide, phosphide and the like, and shows strong basicity. The main components of the carbide slag comprise calcium hydroxide (the mass fraction is 90.1%), silicon oxide (the mass fraction is 3.5%), aluminum oxide (the mass fraction is 2.5%) and a small amount of impurities such as calcium carbonate, ferric oxide, magnesium oxide, titanium dioxide, carbon slag, calcium sulfide and the like. Carbide slag is grey and associated with a pungent smell.
Because the carbide slag amount directly utilized by local production enterprises is limited, the transregional utilization and transportation cost of the low-value material is high, the utilization technical conditions and the technical level of the carbide slag are limited, and a large amount of discharged carbide slag is not effectively utilized. The discharged carbide slag seriously pollutes farmlands and underground water, pollutes the environment and harms human health.
In addition, the tail gas of the lime kiln and the calcium carbide furnace gas of the factory are sulfur-containing flue gas, the potential of preparing the desulfurizer from the calcium carbide slag slurry is very large, and the existing desulfurizer prepared from the calcium carbide slag mainly utilizes clear liquid obtained by solid-liquid separation as desulfurization liquid to spray the flue gas or introduce the flue gas into the desulfurization. However, the slag separated from the clear liquid has higher viscosity and higher water content and containsSeed impurities including SiO2、Al2O3、SO3、Fe2O3、K2O、MgO、Na2If the carbide slag is directly calcined into lime, the content of CaO in the product is low and does not meet the quality requirement, so some research and development units, such as patent CN110270432B, "a method for removing non-calcium mineral impurities in the carbide slag", systematically propose a method for removing non-calcium components to promote the full resource utilization of the carbide slag.
Because the components of the carbide slag slurry are complex, the generated carbide slag waste still has more than 10 percent, so that the slag can not be completely absorbed, and most of the carbide slag slurry still adopts a deep burying mode. In addition, CaC still exists in the treatment process2The waste material brings the risk for advanced treatment, and some peculiar smell gas also can spill over in the course of handling and cause secondary pollution, all above all need improve.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a process for preparing a high-efficiency desulfurizer and a byproduct of active calcium oxide by using carbide slag.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process for preparing a high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag comprises the following steps:
1) putting carbide slag obtained by wet acetylene into a hydrocyclone to obtain nearly transparent clear liquid I and more viscous slurry I, taking the clear liquid I as a desulfurizer, and spraying sulfur-containing flue gas to remove sulfur-containing compounds and most of CO in the flue gas2And smoke dust, and the obtained liquid is subdivided, filtered and recycled into a new desulfurizer;
2) adding the slurry I into hydrochloric acid solution in a stirring pool I, stirring strongly, pumping into a filter press, and pressurizing to obtain large insoluble substances and turbid liquid, wherein the large insoluble substances are washed for 2 times by hydrochloric acid, washed for 1 time by water and NH3·H2Cleaning for 2 times by using O, drying in the air, and then carrying out thermal drying to obtain slag containing Si and Ti;
3) mixing the cleaning solution with the turbid solutionAdding into a closed ball mill, adding NH while grinding3·H2Continuing the ball milling reaction for 20-30min until the system viscosity is basically unchanged, and centrifuging to obtain slurry II and clear liquid II, wherein the slurry II is slag containing Fe and Mg;
4) putting the clear liquid II into a stirring pool II, and adding NH4HCO3The solution is stirred strongly for reaction, 200mu of filter cloth is added for filtration to obtain precipitate and filtrate, and the precipitate is washed with water and drained to obtain CaCO3Drying the filter cake by a fluidized bed to remove water, scattering and paving, putting into a lime kiln, and decomposing at 1050 +/-50 ℃ to obtain nano-grade active calcium oxide;
5) putting the filtrate into a sedimentation tank, adding a polyaluminium chloride flocculant, and aging to obtain floccule and clear liquid III, wherein the floccule is sulfur-containing Al slag which contains peculiar smell and needs to be stored in a sealed manner;
6) clear liquid III containing trace amount of H+、K+And Na+NH of (2)4Adding ammonia water into the Cl solution to adjust the pH value to 11, blowing carbon dioxide gas to produce NH4HCO3The solution is used as a substitute reagent of the stirring tank II in the step 4) to form a calcium chloride ammonia water system, and under the assistance of strong stirring, a trace amount of active calcium oxide produced in the step 4) is added at the same time to be used as a crystal nucleus of an initial reaction, so that the CO introduction of the calcium chloride ammonia water system is changed2The defect of uneven fineness caused by too few initial crystal nuclei is changed by the above method, and the ultrafine calcium carbonate particle precipitation is obtained in the clear solution II.
Preferably, the slag material containing Si and Ti obtained in the step 2) can be used as an additive of cement materials or composite ceramics.
Preferably, ammonia water and a small amount of thiocyanic acid are added into the slag containing Fe and Mg obtained in the step 3), and CO is introduced after stirring2And obtaining magnesium carbonate precipitate and an Fe thiocyanate complex solution, wherein the magnesium carbonate precipitate can be used for preparing brine, magnesium oxide and magnesium sulfate, and the Fe thiocyanate complex solution can be used for treating heavy metal wastewater, especially waste liquid of chloroethylene catalytic reaction.
Preferably, the Al slag in the step 5) is added with hydrogen peroxide, decolored and deodorized, the residual colorless floccule is fished, and is drained after being washed, so that the flocculant can be recycled as the polyaluminum chloride flocculant in the step 5), and the sulfate solution produced after the residual sulfur-containing components are oxidized is colorless, odorless and dilute in concentration and can be used as washing water for large insoluble substances, ball mills, precipitates and the Al slag.
Compared with the prior art, the invention has the beneficial effects that:
1. the method analyzes the main components of the carbide slag, gradually reacts to obtain a desulfurizer and a byproduct of active calcium oxide, simultaneously obtains slag containing Si and Ti, slag containing Fe and Mg and slag containing Al, and more finely screens and processes the slag, so that more than 98 percent of the components are practically applied, and finally, the waste slag is basically not generated, thereby providing a systematic platform for the absorption of all the components.
2. NH of the last step in the invention4The Cl solution can also be circularly treated, so that the basic recycling of ammonia is realized, the cost is reduced, and the superfine calcium carbonate precipitate is obtained through pH and crystal nucleus control, thereby providing a path for the subsequent production of superfine nano-grade active calcium oxide;
3. the invention also realizes the basic recycling of water, greatly reduces the production water cost and conforms to the green production standard.
Drawings
FIG. 1 is a process flow diagram (horizontal arrangement) of a process for preparing a high-efficiency desulfurizer and byproduct active calcium oxide from carbide slag according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a process for preparing a high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag comprises the following steps:
1) putting carbide slag obtained by wet acetylene into a hydrocyclone to obtain nearly transparent clear liquid I and more viscous slurry I, wherein the clear liquid I is used as a desulfurizer for sulfur-containing smokeSpraying the gas to remove sulfur compounds and most of CO in the flue gas2And smoke dust, and the obtained liquid is subdivided, filtered and recycled into a new desulfurizer;
2) adding the slurry I into hydrochloric acid solution in a stirring pool I, stirring strongly, pumping into a filter press, and pressurizing to obtain large insoluble substances and turbid liquid, wherein the large insoluble substances are washed for 2 times by hydrochloric acid, washed for 1 time by water and NH3·H2Cleaning for 2 times by using O, drying in the air, and then carrying out thermal drying to obtain slag containing Si and Ti;
3) mixing the cleaning solution and the turbid solution, adding into a closed ball mill, adding NH while grinding3·H2Continuing the ball milling reaction for 20-30min until the system viscosity is basically unchanged, and centrifuging to obtain slurry II and clear liquid II, wherein the slurry II is slag containing Fe and Mg;
4) putting the clear liquid II into a stirring pool II, and adding NH4HCO3The solution is stirred strongly for reaction, 200mu of filter cloth is added for filtration to obtain precipitate and filtrate, and the precipitate is washed with water and drained to obtain CaCO3Drying the filter cake by a fluidized bed to remove water, scattering and paving, putting into a lime kiln, and decomposing at 1050 +/-50 ℃ to obtain nano-grade active calcium oxide;
5) putting the filtrate into a sedimentation tank, adding a polyaluminium chloride flocculant, and aging to obtain floccule and clear liquid III, wherein the floccule is sulfur-containing Al slag which contains peculiar smell and needs to be stored in a sealed manner;
6) clear liquid III containing trace amount of H+、K+And Na+NH of (2)4Adding ammonia water into the Cl solution to adjust the pH value to 11, blowing carbon dioxide gas to produce NH4HCO3The solution is used as a substitute reagent of the stirring tank II in the step 4) to form a calcium chloride ammonia water system, and under the assistance of strong stirring, a trace amount of active calcium oxide produced in the step 4) is added at the same time to be used as a crystal nucleus of an initial reaction, so that the CO introduction of the calcium chloride ammonia water system is changed2The defect of uneven fineness caused by too few initial crystal nuclei is changed by the above method, and the ultrafine calcium carbonate particle precipitation is obtained in the clear solution II.
Reference documents: this is because of CaCl2-NH3·H2The pH value of the O system is only about 10.4, which is obviously less than about 12.5 of the pH value of the lime milk system, namely equivalent to the pH value of the O system [ OH ]-]Only the latter being [ OH-]1/%; weakly acidic CO2Must first react with weakly basic ammonia to form HCO3 -The reaction speed is far lower than that of the lime milk system with strong basicity, which is not beneficial to forming a large number of crystal nuclei at the initial stage of carbonization and is not beneficial to the superfine of calcium carbonate particles.
Use of other materials:
the slag material containing Si and Ti obtained in the step 2) can be used as an additive of cement materials or composite ceramics.
Adding ammonia water and a small amount of thiocyanic acid into the slag containing Fe and Mg obtained in the step 3), stirring, and introducing CO2And obtaining magnesium carbonate precipitate and an Fe thiocyanate complex solution, wherein the magnesium carbonate precipitate can be used for preparing brine, magnesium oxide and magnesium sulfate, and the Fe thiocyanate complex solution can be used for treating heavy metal wastewater, especially waste liquid of chloroethylene catalytic reaction.
Adding hydrogen peroxide into the Al slag in the step 5), decoloring and deodorizing, fishing out the residual colorless floccule, washing with water, draining, and using the floccule as the polyaluminum chloride flocculating agent in the step 5) for recycling, wherein the sulfate solution produced by oxidizing the residual sulfur-containing components is colorless, odorless and dilute in concentration and can be used as washing water for large insoluble substances, a ball mill, precipitates and the Al slag. The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (4)

1. A process for preparing a high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag is characterized by comprising the following steps:
1) putting carbide slag obtained from wet acetylene into a hydrocyclone to obtain nearly transparent clear liquid I and viscous slurry I, wherein the clear liquid I is used as a desulfurizing agent, and the obtained slurry I is subjected to wet acetylene wet separationSpraying sulfur-containing flue gas to remove sulfur-containing compounds and most of CO in the flue gas2And smoke dust, and the obtained liquid is subdivided, filtered and recycled into a new desulfurizer;
2) adding the slurry I into hydrochloric acid solution in a stirring pool I, stirring strongly, pumping into a filter press, and pressurizing to obtain large insoluble substances and turbid liquid, wherein the large insoluble substances are washed for 2 times by hydrochloric acid, washed for 1 time by water and NH3·H2Cleaning for 2 times by using O, drying in the air, and then carrying out thermal drying to obtain slag containing Si and Ti;
3) mixing the cleaning solution and the turbid solution, adding into a closed ball mill, adding NH while grinding3·H2Continuing the ball milling reaction for 20-30min until the system viscosity is basically unchanged, and centrifuging to obtain slurry II and clear liquid II, wherein the slurry II is slag containing Fe and Mg;
4) putting the clear liquid II into a stirring pool II, and adding NH4HCO3The solution is stirred strongly for reaction, 200mu of filter cloth is added for filtration to obtain precipitate and filtrate, and the precipitate is washed with water and drained to obtain CaCO3Drying the filter cake by a fluidized bed to remove water, scattering and paving, putting into a lime kiln, and decomposing at 1050 +/-50 ℃ to obtain nano-grade active calcium oxide;
5) putting the filtrate into a sedimentation tank, adding a polyaluminium chloride flocculant, and aging to obtain floccule and clear liquid III, wherein the floccule is sulfur-containing Al slag which contains peculiar smell and needs to be stored in a sealed manner;
6) clear liquid III containing trace amount of H+、K+And Na+NH of (2)4Adding ammonia water into the Cl solution to adjust the pH value to 11, blowing carbon dioxide gas to produce NH4HCO3The solution is used as a substitute reagent of the stirring tank II in the step 4) to form a calcium chloride ammonia water system, and a trace amount of the active calcium oxide produced in the step 4) is added simultaneously under the assistance of strong stirring to be used as a crystal nucleus of an initial reaction, so that superfine calcium carbonate particle precipitation is obtained in the clear liquid II.
2. The process for preparing the high-efficiency desulfurizer and the byproduct active calcium oxide by using the carbide slag as claimed in claim 1, wherein the slag material containing Si and Ti obtained in the step 2) is used as an additive of cement materials or composite ceramics.
3. The process for preparing a high-efficiency desulfurizer and by-product active calcium oxide by using carbide slag as claimed in claim 1, wherein the slag containing Fe and Mg obtained in the step 3) is added with ammonia water and a small amount of thiocyanic acid, stirred and then introduced with CO2And obtaining magnesium carbonate precipitate and an Fe thiocyanate complex solution, wherein the magnesium carbonate precipitate is used for preparing brine, magnesium oxide and magnesium sulfate, and the Fe thiocyanate complex solution is used for treating heavy metal wastewater, especially waste liquid of vinyl chloride catalytic reaction.
4. The process for preparing high-efficiency desulfurizer and by-product active calcium oxide by using carbide slag as claimed in claim 1, wherein the Al slag in step 5) is added with hydrogen peroxide, decolored and deodorized, the remaining colorless floccule is fished out, and is drained after being washed, and the aluminum polychloride flocculant in step 5) is recycled, while the sulfate solution produced after the remaining sulfur-containing component is oxidized is colorless and odorless, has a dilute concentration, and is used as washing water for large insoluble substances, a ball mill, precipitates and the Al slag.
CN202111558750.7A 2021-12-17 2021-12-17 Process for preparing high-efficiency desulfurizer and byproduct active calcium oxide by using carbide slag Pending CN114210192A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114772625A (en) * 2022-04-12 2022-07-22 四川大学 Method for dissolving out calcium ions in carbide slag and method for mineralizing and storing CO by using calcium ions in carbide slag2Application of co-produced light calcium carbonate

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CN107140671A (en) * 2017-07-12 2017-09-08 雅安晶玉新材料有限公司 A kind of nano-calcium carbonate powder and preparation method thereof
CN109650428A (en) * 2019-02-14 2019-04-19 陕西金泰氯碱化工有限公司 A method of lime and desulfurizing agent are produced simultaneously using carbide slag
CN109694956A (en) * 2019-01-23 2019-04-30 天津赫普菲乐新材料有限公司 A method of separating iron, magnesium and aluminium element from deliming treated carbide slag
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Publication number Priority date Publication date Assignee Title
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CN107140671A (en) * 2017-07-12 2017-09-08 雅安晶玉新材料有限公司 A kind of nano-calcium carbonate powder and preparation method thereof
CN109694956A (en) * 2019-01-23 2019-04-30 天津赫普菲乐新材料有限公司 A method of separating iron, magnesium and aluminium element from deliming treated carbide slag
CN109650428A (en) * 2019-02-14 2019-04-19 陕西金泰氯碱化工有限公司 A method of lime and desulfurizing agent are produced simultaneously using carbide slag
CN113636583A (en) * 2021-09-08 2021-11-12 山西路桥建设集团有限公司 Preparation method of calcium oxide regenerated from carbide slag

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Title
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114772625A (en) * 2022-04-12 2022-07-22 四川大学 Method for dissolving out calcium ions in carbide slag and method for mineralizing and storing CO by using calcium ions in carbide slag2Application of co-produced light calcium carbonate

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