CN103623768A - Calcium-based carbon dioxide adsorbent and preparation method thereof - Google Patents
Calcium-based carbon dioxide adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a calcium-based carbon dioxide adsorbent and a preparation method thereof. The preparation method comprises the steps of taking sodium carbonate and calcium chloride at equal molar weight as raw materials, tween 80 80 and polyethylene glycol as additives, performing reaction and precipitation in an aqueous solution to form an adsorbent precursor, and roasting the adsorbent precursor to form the calcium-based carbon dioxide adsorbent. The calcium-based carbon dioxide adsorbent obtained by the method has a higher vaterite content, and a high reaction rate with carbon dioxide; 80% of total conversion rate can be reached in 10 minutes basically; the energy consumption is greatly reduced; compared with natural limestone and other synthesized calcium-based adsorbents, the calcium-based carbon dioxide adsorbent has a higher conversion rate and a higher recycling rate, can separate a carbon dioxide component from tail gas of a thermal power plant more effectively, and lowers the total operation cost; and the method has the characteristics of simplicity in operation and low cost.
Description
Technical field
The present invention relates to a kind of carbon dioxide absorber and preparation method thereof, especially a kind of calcium group carbonic anhydride adsorption agent and preparation method thereof.
Background technology
In recent years, the global warming phenomenon causing due to a large amount of discharges of greenhouse gases has caused huge negative effect to the environment of the natural ecosystems of the earth and human survival, as Melting Glaciers:, sea level rise, and natural ecosystems balance is destroyed etc.Carbon dioxide is as topmost greenhouse gases composition, the 280ppm commendable increase of its concentration in atmosphere before by industrial revolution 400ppm so far, the great amount of carbon dioxide discharge that the burning that this main cause is wherein fossil fuel artificially produces.Based on the current national conditions of China, coal remains the one-level energy being widely used most.Because coal has higher C/Hratio, make it in combustion process, also can discharge relatively a large amount of carbon dioxide.In China, power industry is in all CO2 emissions source topmost one, and its discharge capacity reaches the over half of the total discharge of the artificial carbon dioxide of China, and the carbon dioxide that wherein Coal Energy Source produces occupies 97.7% discharge capacity (Zhang, M., Liu, X., Wang, W.W., Zhou, M., Energy Policy, 2013,52,159-165.).Therefore, being conceived to the carbon dioxide capture of coal electricity industry, is to reduce the effective approach of the artificial carbon dioxide total release of China.
Comparatively ripe collecting carbonic anhydride technology is divided into two large classes at present: physisorphtion and chemical absorption method.From feature and the technology maturity of China's conventional thermal power plant flue gas, chemical absorption method is more suitable for the carbon dioxide capture after thermal power plant's burning.In chemical absorption method, adsorbent used is divided into again liquid absorbent and solid absorbent.The tool Typical Representative feature of liquid absorbent is alkanolamine solution, and the existing developing history that surpasses 60 years of technique is relatively ripe and used by a commercialization conventional art.But for reducing costs, save improving constantly of energy consumption aspect requirement, alkanolamine solution method of trapping can not meet the demand of industrial aspect gradually due in recent years.Meanwhile, the calcium oxide-based solid kind adsorbent as master of take more and more causes people's interest and attention, and this type of adsorbent and carbon capture method have low cost, simple operation and other advantages, therefore must become the developing direction of following carbon dioxide capture technology.
The technology of calcium oxide-based Capture by Sorbents carbon dioxide is mainly the thought (Calcium Carbonate Looping) based on Calcium Carbonate Cyclic, with the chemical reaction of carbon dioxide, carbon dioxide is separated from flue gas by adsorbent, then under carbon dioxide enriched environment by absorption product high-temperature calcination, obtain the carbon dioxide of high concentration, so compress again, transportation and storage work.Technique early-stage Study, mainly in natural limestone, because it has cheap, widely distributed feature, and is used in a large number; Yet, restriction due to the architectural characteristic of natural limestone own, cause it when recycling, absorption conversion ratio (absorbing calcium oxide-based adsorbent/adsorbent total amount of the conversion ratio=calcium carbonate that is converted into) for carbon dioxide acutely declines along with the increase of cycle-index, thereby has greatly increased cost absorption.In recent years, increasing researcher starts to pay close attention to the modification work of calcium oxide base class adsorbent, thereby improves it to the absorptivity of carbon dioxide (conversion ratio of natural limestone is about 60%) and the rate that can be recycled.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of calcium group carbonic anhydride adsorption agent with higher absorption conversion ratio and reusable edible rate and preparation method thereof.
For solving the problems of the technologies described above, the technical scheme that the inventive method is taked is: it take equimolar amounts sodium carbonate and calcium chloride is raw material, and Tween 80 and polyethylene glycol, as additive, jointly react and separate out in the aqueous solution, obtain sorbent precursor body; Sorbent precursor body, through calcining, can obtain calcium group carbonic anhydride adsorption agent.
Described in the inventive method, the relative molecular mass of polyethylene glycol is 2000～10000.
The calcium carbonate product that described in the inventive method, reaction generates and the mass ratio of applied Tween 80 are 1:2～1:16; The mass ratio of the calcium carbonate product that reaction generates and polyethylene glycol used is 1:0.5～1:2.
Reaction temperature described in the inventive method is controlled at 20～35 ℃.
Described in the inventive method, calcining is carried out under inert atmosphere; Calcining heat is 800～1000 ℃, and calcination time is 4～8min.
The inventive method is first added to the water Tween 80 and polyethylene glycol, forms mixed solution; Under stirring, to splashing into sodium carbonate liquor in mixed solution and calcium chloride solution reacts; The sediment that reaction generates is separated, dry, obtains sorbent precursor body.
Described in the inventive method, sodium carbonate liquor and calcium chloride solution concentration are 0.01～0.1mol/L.
Described in the inventive method be separated into standing 20～30 hours after Separation of Solid and Liquid.
Baking temperature described in the inventive method is 90～100 ℃, and be 2～3h drying time.
The calcium group carbonic anhydride adsorption agent that the present invention also provides a kind of said method to prepare.
The beneficial effect that adopts technique scheme to produce is: the present invention is from the angle of chemical synthesis, utilize aqueous solution deposition method, and be used in conjunction with Tween 80 and polyethylene glycol as additive, when controlling cost and synthesizing simple and easy degree, to reach best assimilation effect.The present invention obtains calcium group carbonic anhydride adsorption agent and not only has reaction rate faster, and has higher absorption conversion ratio and reusable edible rate; Thereby the efficiency that can effectively improve carbon dioxide capture process, reduces costs.
The calcium group carbonic anhydride adsorption agent that the present invention obtains has higher vaterite content, fast with carbon dioxide reaction speed, substantially can in 10 minutes, reach 80% of total conversion, thus the energy consumption of greatly reducing; Compare with natural limestone, have higher conversion ratio, the carbon dioxide composition in can more effective separated thermal power plant tail gas, has the rate that better can be recycled, thereby reduces the cost of adsorbent raw material.The inventive method has feature simple to operate, with low cost.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further detailed explanation.
Fig. 1 is the low magnifying power SEM figure of calcium group carbonic anhydride adsorption agent presoma of the present invention;
Fig. 2 is the middle magnifying power SEM figure of calcium group carbonic anhydride adsorption agent presoma of the present invention;
Fig. 3 is the high power SEM figure of calcium group carbonic anhydride adsorption agent presoma of the present invention;
Fig. 4 is the XRD figure of calcium group carbonic anhydride adsorption agent presoma of the present invention;
Fig. 5 is calcium group carbonic anhydride adsorption agent of the present invention and the natural limestone comparison schematic diagram of conversion ratio first;
Fig. 6 is calcium group carbonic anhydride adsorption agent of the present invention mass change schematic diagram with cycle-index in TGA;
Fig. 7 is the repeatedly comparison schematic diagram of conversion ratio of calcium group carbonic anhydride adsorption agent of the present invention and natural limestone.
The specific embodiment
Example 1: this calcium group carbonic anhydride adsorption agent adopts following technique to be prepared from.
(1) at ambient temperature, 2g Tween 80 (English: Tween 80 or Polysorbate 80) and 0.25g polyethylene glycol (molecular mass 10000) are joined in the beaker that fills 200ml deionized water, keep even rotating speed 400rpm to stir 5 minutes, solute is fully dissolved in solute.Under 30 ℃ of conditions, 25ml sodium carbonate concentrated solution (0.1mol/L) is slowly splashed in beaker before, subsequently 25ml calcium chloride concentrated solution (0.1mol/L) is slowly splashed in mixed solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Then by beaker standing 24 hours at ambient temperature.In said process, in solution, calcium carbonate product weight is 0.235g; The mass ratio of calcium carbonate product and Tween 80 is 1:8.51, and the mass ratio of calcium carbonate product and polyethylene glycol is 1:1.06.
(2) sediment in beaker is carried out to suction filtration to arrive the object of the organic solvent in abundant eccysis solution.Deposit by filter paper synsedimentary in filter paper surface carefully takes out from filter, is placed in baking oven, keeps 95 degrees Celsius of constant temperature to be dried 2 hours, obtains sorbent precursor body.
(3) sorbent precursor body is calcined 5 minutes in lower 900 degrees Celsius of nitrogen environment, obtained final synthetic calcium group carbonic anhydride adsorption agent.
This example adsorbent is for the method for testing of carbon dioxide absorption rate: adopt thermogravimetric analyzer (TGA), 900 degrees Celsius of calcinings, obtain after calcium oxide-based adsorbent, temperature is dropped to 650 degrees Celsius with the speed of 100 centigrade per minutes, gas is switched to the mist of 15% carbon dioxide 85% nitrogen simultaneously, by the object of this gas, it is the real content for carbon dioxide in simulated fire power-plant flue gas, this reaction continues 60 minutes, now by adsorbent mass, change known its and from calcium oxide, be converted into the conversion ratio of calcium carbonate, be that adsorbent is for the absorption efficiency of carbon dioxide, question response finishes, and temperature is risen to 900 degree with 100 degree speed per minute, gas is switched to nitrogen simultaneously, this temperature lower calcination 5 minutes, thereby again obtains calcium oxide-based adsorbent, above two steps are constantly circulated, just can measure adsorbent in the condition of absorption efficiency and renewable rate repeatedly recycle under to(for) carbon dioxide.
Example 2: this calcium group carbonic anhydride adsorption agent adopts following technique to be prepared from.
(1) at ambient temperature, 3g Tween 80 and 0.25g polyethylene glycol (molecular mass 6000) are joined in the beaker that fills 200ml deionized water, keep even rotating speed 400rpm to stir 5 minutes, solute is fully dissolved in solute.Under 20 ℃ of conditions, in beaker before 50ml sodium carbonate concentrated solution (0.05mol/L) is slowly joined, subsequently 50ml calcium chloride concentrated solution (0.05mol/L) is slowly splashed in mixed solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Then by beaker standing 20 hours at ambient temperature.In said process, in solution, calcium carbonate product weight is 0.240g; The mass ratio of calcium carbonate product and Tween 80 is 1:12.5, and the mass ratio of calcium carbonate product and polyethylene glycol is 1:1.04.
(2) sediment in beaker is carried out to suction filtration to arrive the object of the organic solvent in abundant eccysis solution.Deposit by filter paper synsedimentary in filter paper surface carefully takes out from filter, is placed in baking oven, keeps 95 degrees Celsius of constant temperature to be dried 3 hours, obtains sorbent precursor body.
(3) sorbent precursor body is calcined 4 minutes in lower 1000 degrees Celsius of nitrogen environment, obtained finally synthesizing calcium group carbonic anhydride adsorption agent.
Example 3: this calcium group carbonic anhydride adsorption agent adopts following technique to be prepared from.
(1) at ambient temperature, 3.88g Tween 80 and 0.25g polyethylene glycol (molecular mass 8000) are joined in the beaker that fills 200ml deionized water, keep even rotating speed 400rpm to stir 5 minutes, solute is fully dissolved in solute.Under 35 ℃ of conditions, in beaker before 25ml sodium carbonate concentrated solution (0.1mol/L) is slowly joined, subsequently 25ml calcium chloride concentrated solution (0.1mol/L) is slowly splashed in solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; By beaker standing 30 hours at ambient temperature.In said process, in solution, calcium carbonate product weight is 0.243g; The mass ratio of calcium carbonate product and Tween 80 is 1:16, and the mass ratio of calcium carbonate product and polyethylene glycol is 1:1.03.
(2) sediment in beaker is carried out to suction filtration to arrive the object of the organic solvent in abundant eccysis solution.Deposit by filter paper synsedimentary in filter paper surface carefully takes out from filter, is placed in baking oven, keeps 95 degrees Celsius of constant temperature to be dried 2.5 hours, obtains sorbent precursor body.
(3) sorbent precursor body is calcined 5 minutes in lower 900 degrees Celsius of nitrogen environment, obtained final synthetic calcium group carbonic anhydride adsorption agent.
Example 4: this calcium group carbonic anhydride adsorption agent adopts following technique to be prepared from.
(1) at ambient temperature, 0.48g Tween 80 and 0.47g polyethylene glycol (molecular mass 2000) are joined in the beaker that fills 200ml deionized water, be stirred to solute and be fully dissolved in solute.Under 25 ℃ of conditions, in beaker before 250ml sodium carbonate concentrated solution (0.01mol/L) is slowly joined, subsequently 250ml calcium chloride concentrated solution (0.01mol/L) is slowly splashed in solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; By beaker standing 25 hours at ambient temperature.In said process, in solution, calcium carbonate product weight is 0.239g; The mass ratio of calcium carbonate product and Tween 80 is 1:2, and the mass ratio of calcium carbonate product and polyethylene glycol is 1:2.
(2) sediment in beaker is carried out to suction filtration to arrive the object of the organic solvent in abundant eccysis solution.Deposit by filter paper synsedimentary in filter paper surface carefully takes out from filter, is placed in baking oven, keeps 95 degrees Celsius of constant temperature to be dried 2.5 hours, obtains sorbent precursor body.
(3) sorbent precursor body is calcined 8 minutes in lower 900 degrees Celsius of nitrogen environment, obtained final synthetic calcium group carbonic anhydride adsorption agent.
Example 5: this calcium group carbonic anhydride adsorption agent adopts following technique to be prepared from.
(1) at ambient temperature, 1.5g Tween 80 and 0.123g polyethylene glycol (molecular mass 4000) are joined in the beaker that fills 200ml deionized water, be stirred to solute and be fully dissolved in solute.Under 25 ℃ of conditions, in beaker before 250ml sodium carbonate concentrated solution (0.01mol/L) is slowly joined, subsequently 250ml calcium chloride concentrated solution (0.01mol/L) is slowly splashed in solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; By beaker standing 25 hours at ambient temperature.In said process, in solution, calcium carbonate product weight is 0.246g; The mass ratio of calcium carbonate product and Tween 80 is 1:6.1, and the mass ratio of calcium carbonate product and polyethylene glycol is 1:0.5.
(2) sediment in beaker is carried out to suction filtration to arrive the object of the organic solvent in abundant eccysis solution.Deposit by filter paper synsedimentary in filter paper surface carefully takes out from filter, is placed in baking oven, keeps 95 degrees Celsius of constant temperature to be dried 2.5 hours, obtains sorbent precursor body.
(3) sorbent precursor body is calcined 6 minutes in lower 800 degrees Celsius of nitrogen environment, obtained final synthetic calcium group carbonic anhydride adsorption agent.
Fig. 1, Fig. 2 and Fig. 3 are the low magnifying power of example 1 gained presoma, middle magnifying power and high power SEM figure; All particles are equal equal diameter spherical structure as can be seen from Figure 1, from Fig. 2 and Fig. 3, can find out that spheroidal particle surface is comprised of nanoscale granule; This structure has effectively increased the contact area of carbon dioxide and adsorbent surface, thereby improves absorption efficiency and ability.
Fig. 4 is X-ray polycrystalline diffraction (XRD) figure of example 1 gained sorbent precursor body, and as shown in Figure 4, its chemical composition is mainly calcium carbonate, and main crystal formation is vaterite and calcite, and forerunner's mass ratio more than 90% is vaterite, and only having a small amount of is calcite.
Fig. 5 is this calcium group carbonic anhydride adsorption agent and the comparison of natural limestone for 15% carbon dioxide (with 85% nitrogen mixture body) single absorbability; In figure, curve is followed successively by from the top down, the single absorbability curve of example 3 gained adsorbents, example 2 gained adsorbents, example 1 gained adsorbent and natural limestone.As seen from the figure, the conversion ratio of this calcium group carbonic anhydride adsorption agent has been brought up to more than 99% by 60%, and this calcium group carbonic anhydride adsorption agent embodies higher absorption efficiency, can in 10 minutes, reach 80% of total absorptivity.
Fig. 6 is that example 1 gained adsorbent carries out repeatedly the initial data of loop test in TGA, and method of testing is the method for testing of above-mentioned carbon dioxide absorption rate.Fig. 7 has compared example 1 gained adsorbent (Sorb-1) and has showed with the absorbability that natural limestone (Limestone) repeatedly recycles.From Fig. 6 and Fig. 7, this adsorbent has improved absorption number of times and the uptake for carbon dioxide on the whole greatly.
Claims (10)
1. a preparation method for calcium group carbonic anhydride adsorption agent, is characterized in that: it take sodium carbonate and calcium chloride is raw material, and Tween 80 and polyethylene glycol, as additive, jointly react and separate out in the aqueous solution, obtain sorbent precursor body; Sorbent precursor body, through calcining, obtains calcium group carbonic anhydride adsorption agent.
2. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 1, is characterized in that: the relative molecular mass of described polyethylene glycol is 2000～10000.
3. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 1, is characterized in that: the calcium carbonate product that described reaction generates and the mass ratio of applied Tween 80 are 1:2～1:16; The mass ratio of the calcium carbonate product that reaction generates and polyethylene glycol used is 1:0.5～1:2.
4. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 1, is characterized in that: described reaction temperature is controlled at 20～35 ℃.
5. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 1, is characterized in that: described calcining is carried out under inert atmosphere; Calcining heat is 800～1000 ℃, and calcination time is 4～8min.
6. according to the preparation method of the calcium group carbonic anhydride adsorption agent described in claim 1-5 any one, it is characterized in that: Tween 80 and polyethylene glycol are added to the water, form mixed solution; Under stirring, to splashing into sodium carbonate liquor in mixed solution and calcium chloride solution reacts; The sediment that reaction generates is separated, dry, obtains sorbent precursor body.
7. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 6, is characterized in that: described sodium carbonate liquor and calcium chloride solution concentration are 0.01～0.1mol/L.
8. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 6, is characterized in that: described be separated into standing 20～30 hours after Separation of Solid and Liquid.
9. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 6, is characterized in that: described baking temperature is 90～100 ℃, and be 2～3h drying time.
10. a calcium group carbonic anhydride adsorption agent prepared by claim 1-9 any one method.
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| CN107090321A (en) * | 2017-07-04 | 2017-08-25 | 合肥择浚电气设备有限公司 | A kind of biomass marsh gas purifying technique |
| CN107344092A (en) * | 2017-09-08 | 2017-11-14 | 梅庆波 | A kind of preparation method of high temperature resistant type calcium-based ascarite |
| CN111514853A (en) * | 2020-04-30 | 2020-08-11 | 合肥学院 | Preparation method of calcium carbonate-waste coal-based activated carbon composite adsorbent |
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| CN107090321A (en) * | 2017-07-04 | 2017-08-25 | 合肥择浚电气设备有限公司 | A kind of biomass marsh gas purifying technique |
| CN107344092A (en) * | 2017-09-08 | 2017-11-14 | 梅庆波 | A kind of preparation method of high temperature resistant type calcium-based ascarite |
| CN111514853A (en) * | 2020-04-30 | 2020-08-11 | 合肥学院 | Preparation method of calcium carbonate-waste coal-based activated carbon composite adsorbent |
| CN111514853B (en) * | 2020-04-30 | 2022-08-26 | 合肥学院 | Preparation method of calcium carbonate-waste coal-based activated carbon composite adsorbent |
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