CN115215624B - Carbon dioxide geological sequestration method using phosphogypsum as filler - Google Patents
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- CN115215624B CN115215624B CN202210602628.3A CN202210602628A CN115215624B CN 115215624 B CN115215624 B CN 115215624B CN 202210602628 A CN202210602628 A CN 202210602628A CN 115215624 B CN115215624 B CN 115215624B
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- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/14—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements
- C04B28/142—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements
- C04B28/143—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing calcium sulfate cements containing synthetic or waste calcium sulfate cements the synthetic calcium sulfate being phosphogypsum
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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
- B01D53/14—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 by absorption
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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
- B01D53/46—Removing components of defined structure
- B01D53/62—Carbon oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
- B01D2252/10—Inorganic absorbents
- B01D2252/102—Ammonia
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- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
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- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00724—Uses not provided for elsewhere in C04B2111/00 in mining operations, e.g. for backfilling; in making tunnels or galleries
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Abstract
The invention discloses a carbon dioxide geological sequestration method taking phosphogypsum as a filling material, which comprises the following steps: (1) Placing water, zirconia balls, anhydrous phosphogypsum, cement, red mud and grinding aid into a wet mill for grinding, and screening out slurry; (2) Mixing and stirring the slurry, alkali and phosphate tailings to obtain a filling material; (3) Filling the filling material into the mine goaf through a filling pump; (4) CO is introduced into the inner partition of the filling area 2 The reaction is complete. The invention innovates a mine filling and carbon fixing integrated method, the wet milling method and red mud carbonization are helpful for activating phosphogypsum carbonization reaction activity, the method is simple and easy to implement, the operation is convenient, a large amount of phosphate tailing sand can be consumed, the problem of low utilization rate of phosphogypsum in China for a long time is solved, and a large amount of CO is absorbed in the curing process 2 Is more environment-friendly.
Description
Technical Field
The invention relates to the field of solid waste material treatment, in particular to a carbon dioxide geological storage method taking phosphogypsum as a filling material.
Background
The population of China is numerous, the mineral demand is very high, the mineral reserve of China is huge, and the mining industry is subjected to full-scale period. In recent years, the mineral situation in China has changed greatly, and the mineral industry is developing toward health. The rapid development in the past leaves a lot of problems, wherein goafs are easy to form connected and complex goafs, the life and property safety of people is affected, and meanwhile, irreparable losses are caused to land resources and natural environments. On the other hand, the accumulation of tailings and mining byproducts seriously damages the natural environment, occupies land resources, and is urgent to treat and utilize the accumulated solid wastes such as tailings, mineral solid wastes and the like; phosphogypsum is a byproduct in the production of phosphate fertilizer, has more impurities and lower hydration activity than ordinary phosphogypsum, has low utilization rate of phosphogypsum in China, is piled up, and can effectively treat a large amount of phosphogypsum.
CO at present 2 Global warming by emissions has compromised the ecological balance of all humans and the whole earth, and with increasing levels of industrialization, the situation is becoming more severe. How to combine solid waste with CO 2 The green resource utilization is a key scientific and technical problem to be solved at present.
Disclosure of Invention
The invention aims to provide a method for geological sequestration of carbon dioxide by taking phosphogypsum as a filling material, which aims to solve the problems in the background technology.
The technical scheme of the invention is as follows:
a method for geological sequestration of carbon dioxide with phosphogypsum as a filler, comprising:
(1) 100 to 200 parts by mass of water, 200 parts by mass of zirconia balls, 60 to 90 parts by mass of anhydrous phosphogypsum, 5 to 20 parts by mass of cement, 5 to 20 parts by mass of red mud and 1 to 2 parts by mass of grinding aid are put into a wet mill to be ground for 40 to 60 minutes, and slurry is sieved;
(2) Mixing and stirring the slurry, 10-20 parts by mass of alkali and phosphate tailings to obtain a filling material, wherein the glue sand ratio is 1:8-1:14, sand is phosphate tailings, and the cementing material comprises anhydrous phosphogypsum, cement and red mud;
(3) Filling the filling material into the mine goaf through a filling pump;
(4) CO is introduced into the filling area at a flow rate of 1 to 2 parts by mass/min 2 The gas undergoes a calcium reaction. CO is introduced into the invention 2 Gas, CO 2 The gas and the filling material are subjected to calcium mineralization reaction.
The preferred scheme of the method is as follows:
(1) 100 to 150 parts by mass of water, 200 parts by mass of zirconia balls, 60 to 80 parts by mass of anhydrous phosphogypsum, 10 to 20 parts by mass of cement, 10 to 20 parts by mass of red mud and 1 to 2 parts by mass of grinding aid are put into a wet mill to be ground for 40 to 60 minutes, and slurry is sieved;
(2) Mixing and stirring the slurry, 10-20 parts by mass of alkali and phosphate tailings to obtain a filling material, wherein the glue sand ratio is 1:8-1:10, sand is phosphate tailings, and the cementing material comprises anhydrous phosphogypsum, cement and red mud;
(3) Filling the filling material into the mine goaf through a filling pump;
(4) CO is introduced into the filling area at a flow rate of 1 to 2 parts by mass/min 2 And (3) reacting the gas.
Further, the glue sand ratio in the step (2) is preferably 1:8-1:9.
In some embodiments, in step (4), the CO is delivered by movement 2 The gas outlet of the gas pipeline controls the residence time of the gas outlet in the filling material in unit volume, and controls the residence time in the filling material in unit volume to reach 5-7 h, namely the carbon mineralization time; the unit volume refers to 1 cubic meter.
Further, when the residence time in the unit volume of the filling material reaches 5-7 hours, whether the CO is stopped to be fed or not is further judged 2 The method specifically comprises the following steps:
monitoring the pH value of the filling material, and stopping introducing CO when the pH value is monitored to be constant 2 The method comprises the steps of carrying out a first treatment on the surface of the After waiting for 5-10 min, monitoring the pH value of the filling again, wherein the pH value is still constant, and the full reaction is indicated; otherwise, continuing to introduce CO 2 。
In some embodiments, the grinding aid is triethanolamine.
In some embodiments, in step (1), the wet mill is liquid phase milled at a rate of 400r/min for 40-60 minutes.
In some embodiments, the anhydrous phosphogypsum median particle size is preferably less than 35 μm.
In some embodiments, the red mud median particle size is preferably less than 5 μm.
In some embodiments, the base is one or a mixture of ammonia and sodium hydroxide.
In some embodiments, the phosphate tailings are phosphate tailings sand with a water content of no more than 7.5% and a particle size of 10 μm to 90 μm.
The invention mixes anhydrous phosphogypsum, red mud and phosphate tailings, fills the goaf, and then introduces CO 2 Gas, CO 2 After being introduced, the calcium sulfate reacts with CO in alkaline environment 2 The reaction generates calcium carbonate, and certain strength is formed. Meanwhile, sodium carbonate generated by carbonization of the red mud can be used as an exciting agent to excite the reactivity of the anhydrous phosphogypsum. Finally, solid waste materials and CO 2 The goaf sealing device has certain strength and meets the normal activity requirement of the upper part of the goaf. The obtained filling system achieves three purposes of solid waste treatment, mining area filling and carbon sequestration at the same time, and has wide application prospect.
The invention takes phosphogypsum as the main component of the filling material, and solid waste slurry such as phosphogypsum treated by wet grinding has the characteristics of uniform distribution, large specific surface area of particles and sufficient ion dissolution, and the alkali such as ammonia water and the like is added on the basis, and then CO is introduced 2 The carbonic acid precipitate can be formed later to form certain strength, which is helpful for geological stability; the invention well combines two technologies of texture sealing and carbon dioxide mineralization, and achieves win-win of solid waste treatment and carbon fixation.
The invention has the following advantages and beneficial effects:
1. the filling material provided by the invention is prepared from solid wastes such as phosphogypsum, red mud, phosphate tailings and the like, can absorb a large amount of piled solid wastes, is a green filling material, and is an effective utilization way for solving the problem that the solid wastes occupy land resources in long-term piling.
2. The filling material is a carbon-fixing cementing material, the filling material is introduced into the slurry through a carbon dioxide gas partition of a gas transmission pipeline after a goaf is pumped, phosphogypsum can react with carbon dioxide in a carbon mineralization way under an alkaline environment so as to fix the carbon dioxide, and an economic and feasible route is provided for a carbon dioxide solidification and sealing technology.
3. The invention adopts the liquid phase grinding technology to treat the cementing material used for filling, optimizes the particle shape of the solid waste in the grinding process, is beneficial to the filling effect, promotes more ions (such as calcium, silicon, aluminum, sulfate radical and the like) to be dissolved out, improves the carbonization and hydration reaction activities of the solid waste, and further improves the carbon conversion rate and the strength of the filling body.
Detailed Description
For a better understanding of the present invention, the following examples are further illustrative of the present invention, but the content of the present invention is not limited to the following examples.
In the embodiment, silicate PI 42.5 cement is selected as the cement; phosphogypsum is from the solid waste discharged from the suitable Hubei, and the median particle size is 30 mu m; the red mud is discharged solid waste from Henan Hengyuan aluminum industry, and the median particle size is 150 mu m; triethanolamine is selected as a grinding aid; the median particle diameter of the phosphate tailing sand is 80 mu m, and the water content is 3%; the alkali is ammonia water.
Example 1
The specific steps of this embodiment are as follows:
(1) 100 parts by mass of water, 200 parts by mass of zirconia balls with the sphere diameter of 2.0-2.5 mm, 60 parts by mass of anhydrous phosphogypsum, 20 parts by mass of cement, 20 parts by mass of red mud and 1 part by mass of triethanolamine are mixed, placed into a wet mill, subjected to liquid-phase grinding for 40min, and sieved to obtain slurry, and the particle size of the slurry is measured by a laser particle sizer and is shown in table 1.
(2) And (3) placing the slurry obtained in the step (1), 10 parts by mass of ammonia water and 800 parts by mass of phosphate tailings into a stirrer to be uniformly stirred to obtain a filling material, and performing expansion test on the filling material according to GB/T50119-2016 'concrete admixture application technical Specification', wherein the expansion test is shown in table 1.
(3) CO is introduced into the filling material 2 The gas is subjected to carbon mineralization reaction, the gas speed is 1 part by mass/min, the pH value is measured every 5min, and when the pH value of the filling material is constant, CO is stopped being introduced 2 The method comprises the steps of carrying out a first treatment on the surface of the After 5min, the pH was measured again, and a constant value was considered to be the completion of the mineralization reaction, from which the carbon conversion and the carbon conversion efficiency were calculated.
(4) And taking a cubic sample from the slurry after the carbon mineralization is completed, and carrying out the tests of the shrinkage rate and the compressive strength of the standard cube after standard maintenance for 28d, wherein the test of the shrinkage rate refers to the standard JC/T2478-2018 of tail sand concrete for filling a mine goaf, and the test of the compressive strength refers to the standard GB/T17671-2021 of cement mortar strength test method.
Example 2
The specific steps of this embodiment are as follows:
(1) 150 parts by mass of water, 200 parts by mass of zirconia balls with the sphere diameter of 2.0-2.5 mm, 80 parts by mass of phosphogypsum, 10 parts by mass of cement, 10 parts by mass of red mud and 1.5 parts by mass of triethanolamine are mixed, placed into a wet mill, subjected to liquid-phase grinding for 40min, and sieved to obtain slurry, and the particle size of the slurry is measured by a laser particle sizer and is shown in table 1.
(2) And (3) placing the slurry obtained in the step (1), 15 parts by mass of ammonia water and 1000 parts by mass of phosphate tailings into a stirrer to be uniformly stirred to obtain a filling material, and performing expansion degree test on the filling material, wherein the test result is shown in Table 1.
(3) CO is introduced into the filling material 2 The gas is subjected to carbon mineralization reaction, the gas speed is 1.5 parts by mass/min, the pH value is measured every 5min, and when the pH value of the filling material is constant, CO is stopped being introduced 2 After 5min, the pH was measured again, and a constant value was considered to be the completion of the carbon mineralization reaction, from which the carbon conversion and the carbon conversion efficiency were calculated.
(4) And taking a cubic sample from the slurry after the carbon mineralization is completed, and carrying out tests on the shrinkage rate and the compressive strength of a standard cube after standard curing for 28 days.
Example 3
(1) 200 parts by mass of water, 200 parts by mass of zirconia balls with the sphere diameter of 2.0-2.5 mm, 90 parts by mass of phosphogypsum, 5 parts by mass of cement, 5 parts by mass of red mud and 1.5 parts by mass of triethanolamine are mixed, placed into a wet mill, subjected to liquid-phase grinding for 60min, and sieved to obtain slurry, and the particle size of the slurry is measured by a laser particle sizer and is shown in table 1.
(2) And (3) placing the slurry obtained in the step (1), 20 parts by mass of ammonia water and 1400 parts by mass of phosphate tailings into a stirrer to be uniformly stirred to obtain a filling material, and performing expansion degree test on the filling material, wherein the test result is shown in table 1.
(3) CO is introduced into the filling material 2 The gas is subjected to carbon mineralization reaction, the gas speed is 2 parts by mass/min, the pH value is measured every 5min, and the gas is used as filling materialStopping CO feeding at constant pH 2 After 5min, the pH was measured again, and a constant value was considered to be the completion of the carbon mineralization reaction, from which the carbon conversion and the carbon conversion efficiency were calculated.
(4) And taking a cubic sample from the slurry after the carbon mineralization is completed, and carrying out tests on the shrinkage rate and the compressive strength of a standard cube after standard curing for 28 days.
Example 4
(1) 150 parts by mass of water, 200 parts by mass of zirconia balls with the sphere diameter of 2.0-2.5 mm, 80 parts by mass of phosphogypsum, 10 parts by mass of cement, 10 parts by mass of red mud and 2 parts by mass of triethanolamine are mixed, placed in a wet mill, subjected to liquid-phase grinding for 60min, and screened to obtain slurry, and the particle size of the slurry is measured by a laser particle sizer, and is shown in table 1.
(2) And (3) placing the slurry obtained in the step (1), 20 parts by mass of ammonia water and 900 parts by mass of phosphate tailings into a stirrer to be uniformly stirred to obtain a filling material, and performing expansion degree test on the filling material, wherein the test result is shown in table 1.
(3) CO is introduced into the filling material 2 The gas is subjected to carbon mineralization reaction, the gas speed is 2 parts by mass/min, the pH value is measured every 5min, and when the pH value of the filling material is constant, CO is stopped being introduced 2 After 5min, the pH was measured again, and a constant value was considered to be the completion of the carbon mineralization reaction, from which the carbon conversion and the carbon conversion efficiency were calculated.
(4) And taking a cubic sample from the slurry after the carbon mineralization is completed, and carrying out tests on the shrinkage rate and the compressive strength of a standard cube after standard curing for 28 days.
TABLE 1 detection data for products of examples 1 to 4
The carbon conversion and the carbon conversion efficiency are calculated from the data of thermogravimetric analysis (TG), wherein the carbon conversion efficiency refers to the mass of carbon dioxide solidified per unit mass of the carbon-fixing material per unit time, in this example referred to as "wet milling slurry". The "parts" in unit parts/(parts) h) of the carbon conversion efficiency means parts by mass.
As can be seen from Table 1, the slurries obtained according to the invention have a median particle size of 1.6 μm to 3.1. Mu.m; the expansion degree of the obtained filling material is 250-310 mm, and the sinking rate is 1.5% -2.5%; the compressive strength of the obtained carbon-fixing filling material after the consolidation is finished for 28 days is 2.1 MPa-3.5 MPa. As can be seen from the table, with optimization of phosphogypsum doping amount and particle diameter, carbon conversion rate and conversion efficiency are improved, but shrinkage index and strength index are deteriorated, so that example 4 is an optimal group, and compressive strength and shrinkage rate meet the national standard of filling materials.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A method for geological sequestration of carbon dioxide using phosphogypsum as a filler, which is characterized by comprising the following steps:
(1) 100 to 200 parts by mass of water, 200 parts by mass of zirconia balls, 60 to 90 parts by mass of anhydrous phosphogypsum, 5 to 20 parts by mass of cement, 5 to 20 parts by mass of red mud and 1 to 2 parts by mass of grinding aid are put into a wet mill to be ground for 40 to 60 minutes, and slurry is sieved;
(2) Mixing and stirring the slurry, 10-20 parts by mass of alkali and phosphate tailings to obtain a filling material, wherein the glue sand ratio is 1:8-1:14, sand is phosphate tailings, and the cementing material comprises anhydrous phosphogypsum, cement and red mud;
(3) Filling the filling material into the mine goaf through a filling pump;
(4) CO is introduced into the filling area at a flow rate of 1 to 2 parts by mass/min 2 And (3) reacting the gas.
2. The phosphogypsum-filled carbon dioxide geological sequestration method as claimed in claim 1, comprising:
in the step (1), 100-150 parts by mass of water, 60-80 parts by mass of anhydrous phosphogypsum, 10-20 parts by mass of cement and 10-20 parts by mass of red mud; and the glue sand ratio in the step (2) is 1:8-1:10.
3. The phosphogypsum-filled carbon dioxide geological sequestration method as claimed in claim 2, wherein:
the glue sand ratio is 1:8-1:9.
4. A method of carbon dioxide geological sequestration filled with phosphogypsum as claimed in any one of claims 1 to 3, characterised in that:
in step (4), CO is conveyed by moving 2 And the gas outlet of the gas pipeline controls the residence time of the gas outlet in the filling material in unit volume and controls the residence time in the filling material in unit volume to be 5-7 h.
5. The phosphogypsum-filled carbon dioxide geological sequestration method as claimed in claim 4, wherein:
when the residence time in the filling material in unit volume reaches 5-7 h, further judging whether to stop introducing CO 2 : monitoring the pH value of the filling material, and stopping introducing CO when the pH value is monitored to be constant 2 The method comprises the steps of carrying out a first treatment on the surface of the After waiting for 5-10 min, monitoring the pH value of the filling again, wherein the pH value is still constant, and the full reaction is indicated; otherwise, continuing to introduce CO 2 。
6. A method of carbon dioxide geological sequestration filled with phosphogypsum as claimed in any one of claims 1 to 3, characterised in that:
the grinding aid adopts triethanolamine.
7. A method of carbon dioxide geological sequestration filled with phosphogypsum as claimed in any one of claims 1 to 3, characterised in that:
the median particle diameter of the anhydrous phosphogypsum is less than 35 mu m.
8. A method of carbon dioxide geological sequestration filled with phosphogypsum as claimed in any one of claims 1 to 3, characterised in that:
the median particle size of the red mud is less than 5 mu m.
9. A method of carbon dioxide geological sequestration filled with phosphogypsum as claimed in any one of claims 1 to 3, characterised in that:
the alkali is one or a mixture of two of ammonia water and sodium hydroxide.
10. A method of carbon dioxide geological sequestration filled with phosphogypsum as claimed in any one of claims 1 to 3, characterised in that:
the phosphate tailing adopts phosphate tailing sand, the water content is not more than 7.5%, and the grain diameter is 10-90 mu m.
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| CA2888236A1 (en) * | 2015-04-14 | 2016-10-14 | Syncrude Canada Ltd. | Method for preparing a trafficable tailings deposit |
| CN104891878A (en) * | 2015-05-15 | 2015-09-09 | 河海大学 | Cement based carbon dioxide curing agent and preparation method thereof |
| CN108947435A (en) * | 2018-07-12 | 2018-12-07 | 昆明理工大学 | A kind of filling in mine material and preparation method thereof of cooperative disposal mine heavy metal wastewater thereby |
| CN112279605A (en) * | 2020-10-22 | 2021-01-29 | 湖北工业大学 | Underground filling cementing material and preparation method and application thereof |
| CN113213829A (en) * | 2021-05-21 | 2021-08-06 | 北京科技大学 | Tailing carbonization cemented filling method |
| CN114380518A (en) * | 2022-01-25 | 2022-04-22 | 中国地质大学（武汉） | Bayer process red mud-phosphogypsum baking-free cementing material and preparation method thereof |
| CN114538876A (en) * | 2022-03-21 | 2022-05-27 | 重庆大学 | Mineralization of CO by solid waste of mining industry2Method for preparing mine cemented filling material |
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