CN103623768B - Calcium group carbonic anhydride adsorption agent and preparation method thereof - Google Patents
Calcium group carbonic anhydride adsorption agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of calcium group carbonic anhydride adsorption agent and preparation method thereof, it is with equimolar amounts sodium carbonate and calcium chloride for raw material, and Tween 80 and polyethylene glycol, as additive, react precipitation jointly in aqueous, obtain sorbent precursor body; Sorbent precursor body, through calcining, can obtain calcium group carbonic anhydride adsorption agent.The calcium group carbonic anhydride adsorption agent that this method obtains has higher vaterite content, fast with carbon dioxide reaction speed, substantially can reach 80% of total conversion in 10 minutes, thus greatly reduce energy consumption; Compared with synthesizing Ca-base adsorbent with natural limestone and other, there is higher conversion ratio and recycle rate, can more effectively be separated the dioxide component in thermal power plant's tail gas and reduce overall operation cost; This method has feature simple to operate, with 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 caused due to a large amount of discharge of greenhouse gases has caused huge negative effect to the natural ecosystems of the earth and the environment of human survival, as Melting Glaciers:, sea level rise, and natural ecosystems balance is destroyed etc.Carbon dioxide is as topmost greenhouse gases composition, and its concentration is in an atmosphere by the 280ppm commendable increase 400ppm so far before the industrial revolution, and this main cause is wherein the great amount of carbon dioxide discharge that the burning of fossil fuel artificially produces.Based on the national conditions that China is current, coal remains the one-level energy be widely used most.Because coal has higher C/Hratio, make it also can discharge relatively a large amount of carbon dioxide in combustion.In China, power industry is in all CO2 emission sources topmost one, and it is over half that its discharge capacity reaches that the artificial carbon dioxide of China always discharges, and the carbon dioxide that wherein Coal Energy Source produces occupies discharge capacity (Zhang, M., the Liu of 97.7%, X., Wang, W.W., Zhou, M., EnergyPolicy, 2013,52,159-165.).Therefore, being conceived to the carbon dioxide capture of coal electrical travelling industry, is reduce the effective approach of China's artificial carbon dioxide total release.
Collecting carbonic anhydride technology comparatively ripe is at present divided into two large classes: 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.Adsorbent used in chemical absorption method is divided into again liquid absorbent and solid absorbent.Liquid absorbent most Typical Representative feature is alkanolamine solution, and technique has the developing history more than 60 years, is a relative maturity be commercially used the conventional art of use.But due in recent years for reduce costs, save energy consumption aspect require improve constantly, alkanolamine solution method of trapping can not meet the demand of industrial aspect gradually.Meanwhile, more and more cause interest and the attention of people based on calcium oxide-based solid kind adsorbent, this type of adsorbent and carbon capture method have low cost, simple operation and other advantages, therefore inherently become the developing direction of following carbon dioxide capture technology.
The technology of calcium oxide-based Capture by Sorbents carbon dioxide is mainly based on the thought (CalciumCarbonateLooping) of Calcium Carbonate Cyclic, carbon dioxide is separated from flue gas with the chemical reaction of carbon dioxide by adsorbent, then under carbon dioxide enriched environment by absorption product high-temperature calcination, obtain the carbon dioxide of high concentration, and then carry out again compressing, transporting and storage work.Technique early-stage Study, mainly in natural limestone, because it has cheap, widely distributed feature, and is widely used; But, due to the restriction of the architectural characteristic of natural limestone own, cause it when recycling, sorption enhanced rate (sorption enhanced rate=be converted into the calcium oxide-based adsorbent/adsorbent total amount of calcium carbonate) for carbon dioxide acutely declines along with the increase of cycle-index, thus considerably increases cost absorption.In recent years, increasing researcher starts the modification work paying close attention to calcium oxide base class adsorbent, thus improves its absorptivity to 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 ofly has calcium group carbonic anhydride adsorption agent of higher sorption enhanced rate 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 is with equimolar amounts sodium carbonate and calcium chloride for raw material, and Tween 80 and polyethylene glycol, as additive, react precipitation jointly in aqueous, obtain sorbent precursor body; Sorbent precursor body, through calcining, can obtain calcium group carbonic anhydride adsorption agent.
The relative molecular mass of polyethylene glycol described in the inventive method is 2000 ~ 10000.
The calcium carbonate product reacting generation described in the inventive method is 1:2 ~ 1:16 with the mass ratio of the Tween 80 applied; 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 controls at 20 ~ 35 DEG C.
Calcine described in the inventive method and carry out under an inert atmosphere; Calcining heat is 800 ~ 1000 DEG C, and calcination time is 4 ~ 8min.
Tween 80 and polyethylene glycol are first added to the water by the inventive method, form mixed solution; Under stirring, in mixed solution, instill sodium carbonate liquor and calcium chloride solution reacts; The sediment that reaction generates is separated, drying, obtains sorbent precursor body.
Sodium carbonate liquor described in the inventive method 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 DEG C, and drying time is 2 ~ 3h.
Present invention also offers calcium group carbonic anhydride adsorption agent prepared by a kind of said method.
The beneficial effect adopting technique scheme to produce is: the angle that the present invention chemically synthesizes is set out, utilize aqueous solution deposition method, and with the use of Tween80 and polyethylene glycol as additive, while controlling cost and synthesizing ease, 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 sorption enhanced rate and reusable edible rate; Thus effectively can improve the efficiency of carbon dioxide capture process, reduce 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 reach 80% of total conversion in 10 minutes, thus greatly reduce energy consumption; Compared with natural limestone, there is higher conversion ratio, more effectively can be separated the dioxide component in thermal power plant's tail gas, there is the rate that better can be recycled, thus reduce the cost of adsorbent 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 that the low magnifying power SEM of calcium group carbonic anhydride adsorption agent presoma of the present invention schemes;
Fig. 2 is that the middle magnifying power SEM of calcium group carbonic anhydride adsorption agent presoma of the present invention schemes;
Fig. 3 is that the high power SEM of calcium group carbonic anhydride adsorption agent presoma of the present invention schemes;
Fig. 4 is the XRD figure of calcium group carbonic anhydride adsorption agent presoma of the present invention;
Fig. 5 be calcium group carbonic anhydride adsorption agent of the present invention with natural limestone first conversion ratio compare schematic diagram;
Fig. 6 is calcium group carbonic anhydride adsorption agent of the present invention mass change schematic diagram with cycle-index in TGA;
Fig. 7 be calcium group carbonic anhydride adsorption agent of the present invention with natural limestone repeatedly conversion ratio compare schematic diagram.
Detailed description of the invention
Example 1: this calcium group carbonic anhydride adsorption agent adopts following technique to be prepared from.
(1) at ambient temperature, by 2g Tween 80 (English: Tween80 or Polysorbate80) and 0.25g polyethylene glycol (molecular mass 10000) join in the beaker filling 200ml deionized water, keep even rotating speed 400rpm to stir 5 minutes, solute is fully dissolved in solute.Under 30 DEG C of conditions, in beaker before 25ml sodium carbonate concentrated solution (0.1mol/L) is slowly added dropwise to, subsequently 25ml calcium chloride concentrated solution (0.1mol/L) is slowly added dropwise in mixed solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Then beaker is left standstill 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 suction filtration to arrive the object of the organic solvent in abundant eccysis solution.The deposit of filter paper synsedimentary in its surface is carefully taken out from filter, is placed in baking oven, keep constant temperature 95 degrees Celsius of dryings 2 hours, obtain sorbent precursor body.
(3) sorbent precursor body is calcined 5 minutes in lower 900 degrees Celsius of nitrogen environment, obtain the calcium group carbonic anhydride adsorption agent of final synthesis.
This example adsorbent is for the method for testing of carbon dioxide absorption rate: adopt thermogravimetric analyzer (TGA), after 900 degrees Celsius of calcinings obtain 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 real content that the object of this gas is in order to carbon dioxide in simulated fire power-plant flue gas, this reaction continues 60 minutes, now change known its by adsorbent mass and to be converted into the conversion ratio of calcium carbonate from calcium oxide, namely adsorbent is for the absorption efficiency of carbon dioxide, question response terminates, and temperature is risen to 900 degree with 100 degree of speed per minute, gas is switched to nitrogen simultaneously, calcines 5 minutes at this temperature, thus again obtains calcium oxide-based adsorbent, above two steps are constantly circulated, just can measure adsorbent and repeatedly recycle under condition for the absorption efficiency of carbon dioxide and renewable rate.
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 filling 200ml deionized water, keeps even rotating speed 400rpm to stir 5 minutes, solute is fully dissolved in solute.Under 20 DEG C 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 added dropwise in mixed solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Then beaker is left standstill 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 suction filtration to arrive the object of the organic solvent in abundant eccysis solution.The deposit of filter paper synsedimentary in its surface is carefully taken out from filter, is placed in baking oven, keep constant temperature 95 degrees Celsius of dryings 3 hours, obtain sorbent precursor body.
(3) sorbent precursor body is calcined 4 minutes in lower 1000 degrees Celsius of nitrogen environment, finally synthesized 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 filling 200ml deionized water, keeps even rotating speed 400rpm to stir 5 minutes, solute is fully dissolved in solute.Under 35 DEG C 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 added dropwise in solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Beaker is left standstill 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 suction filtration to arrive the object of the organic solvent in abundant eccysis solution.The deposit of filter paper synsedimentary in its surface is carefully taken out from filter, is placed in baking oven, keep constant temperature 95 degrees Celsius of dryings 2.5 hours, obtain sorbent precursor body.
(3) sorbent precursor body is calcined 5 minutes in lower 900 degrees Celsius of nitrogen environment, obtain the calcium group carbonic anhydride adsorption agent of final synthesis.
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 filling 200ml deionized water, is stirred to solute and is fully dissolved in solute.Under 25 DEG C 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 added dropwise in solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Beaker is left standstill 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 suction filtration to arrive the object of the organic solvent in abundant eccysis solution.The deposit of filter paper synsedimentary in its surface is carefully taken out from filter, is placed in baking oven, keep constant temperature 95 degrees Celsius of dryings 2.5 hours, obtain sorbent precursor body.
(3) sorbent precursor body is calcined 8 minutes in lower 900 degrees Celsius of nitrogen environment, obtain the calcium group carbonic anhydride adsorption agent of final synthesis.
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 filling 200ml deionized water, is stirred to solute and is fully dissolved in solute.Under 25 DEG C 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 added dropwise in solution, now can be observed adularescent sediment and separate out, continue to keep stirring 5 minutes; Beaker is left standstill 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 suction filtration to arrive the object of the organic solvent in abundant eccysis solution.The deposit of filter paper synsedimentary in its surface is carefully taken out from filter, is placed in baking oven, keep constant temperature 95 degrees Celsius of dryings 2.5 hours, obtain sorbent precursor body.
(3) sorbent precursor body is calcined 6 minutes in lower 800 degrees Celsius of nitrogen environment, obtain the calcium group carbonic anhydride adsorption agent of final synthesis.
Fig. 1, Fig. 2 and Fig. 3 are that the low magnifying power of example 1 gained presoma, middle magnifying power and high power SEM scheme; All particles are impartial diameter spherical structure as can be seen from Figure 1, can find out that spheroidal particle surface is made up of nanoscale granule from Fig. 2 and Fig. 3; This structure effectively increases the contact area of carbon dioxide and adsorbent surface, thus 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 natural limestone comparing for 15% carbon dioxide (with 85% nitrogen mixed gas) single absorbability; In figure, curve is followed successively by from the top down, the single absorbability curve of example 3 gained adsorbent, example 2 gained adsorbent, example 1 gained adsorbent and natural limestone.As seen from the figure, the conversion ratio of this calcium group carbonic anhydride adsorption agent has brought up to more than 99% by 60%, and this calcium group carbonic anhydride adsorption agent embodies higher absorption efficiency, can reach 80% of total absorptivity in 10 minutes.
Fig. 6 is the initial data that example 1 gained adsorbent carries out repeatedly loop test in TGA, and method of testing is the method for testing of above-mentioned carbon dioxide absorption rate.Fig. 7 compares the absorbability that example 1 gained adsorbent (Sorb-1) and natural limestone (Limestone) repeatedly recycle and shows.From Fig. 6 and Fig. 7, this adsorbent substantially increases absorption number of times for carbon dioxide and uptake on the whole.
Claims (3)
1. a preparation method for calcium group carbonic anhydride adsorption agent, is characterized in that: it is with sodium carbonate and calcium chloride for raw material, and Tween 80 and polyethylene glycol, as additive, react precipitation jointly in aqueous, obtain sorbent precursor body; Sorbent precursor body, through calcining, obtains calcium group carbonic anhydride adsorption agent; The relative molecular mass of described polyethylene glycol is 2000 ~ 10000; The calcium carbonate product that described reaction generates is 1:2 ~ 1:16 with the mass ratio of the Tween 80 applied; The mass ratio of the calcium carbonate product that reaction generates and polyethylene glycol used is 1:0.5 ~ 1:2; Described reaction temperature controls at 20 ~ 35 DEG C; Described calcining is carried out under an inert atmosphere; Calcining heat is 800 ~ 1000 DEG C, and calcination time is 4 ~ 8min; Tween 80 and polyethylene glycol are added to the water, form mixed solution; Under stirring, in mixed solution, instill sodium carbonate liquor and calcium chloride solution reacts; The sediment that reaction generates is separated, drying, obtains sorbent precursor body; Described sodium carbonate liquor and calcium chloride solution concentration are 0.01 ~ 0.1mol/L; Described be separated into standing 20 ~ 30 hours after Separation of Solid and Liquid.
2. the preparation method of calcium group carbonic anhydride adsorption agent according to claim 1, is characterized in that: described baking temperature is 90 ~ 100 DEG C, and drying time is 2 ~ 3h.
3. the calcium group carbonic anhydride adsorption agent prepared of claim 1 or 2 method.
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