CN105461305A - Preparation method of ceramic composite material for adsorbing carbon dioxide - Google Patents
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Abstract
The invention relates to a preparation method of a ceramic composite material for adsorbing carbon dioxide, and belongs to the technical field of adsorbing material preparation. The preparation method comprises the steps that firstly, cinnamomum kotoense roots and stems which are cleaned up are placed in a drying oven to be dried and then extruded into blocks, and carbonizing, smashing and screening are performed to obtain carbonization powder for standby application; secondly, materials such as titanium dioxide and niobium pentoxide are mixed and then placed in a calcining furnace to be calcined, and temperature lowering and grinding are performed to obtain a ceramic substrate; thirdly, the ceramic substrate is evenly mixed with the materials such as the carbonization powder, and then ultrasonic oscillating, calcining, cooling, quenching and temperature lowering are performed. The preparation method has the advantages that the prepared ceramic composite material for adsorbing the carbon dioxide is good in adsorption property, the adsorption efficiency is increased by 10%-15%, repeated cyclic utilization is achieved, and secondary pollution cannot be caused to the environment.
Description
Technical field
The present invention relates to a kind of preparation method for absorbing carbon dioxide ceramic composite, belong to technical field of adsorption material preparation.
Background technology
At present, the fossil oil such as coal and oil accounts for and consumes more than 85% of the energy in the world at present.In this century, this class A fuel A still dominate.But the burning of fossil oil is a large amount of carbonic acid gas to airborne release but, makes atmospheric layer form fearful Greenhouse effect, brings disastrous effect to the living environment of the mankind.Therefore, the discharge of effective technical controlling carbonic acid gas must be developed, and the exploitation of sorbent material to carbonic acid gas highly selective and high-adsorption-capacity, there is important theory significance and practical significance undoubtedly.
At present, conventional carbonic acid gas physisorption material such as zeolite, gac have larger loading capacity to carbonic acid gas at low temperatures, but poor to the selectivity of carbonic acid gas when there being other gases to exist, and when temperature is higher than 30 DEG C, its adsorptive capacity declines obviously.Chemical absorption demonstrates higher selective absorbing to carbonic acid gas.At present, the sorbent material for chemical absorption carbonic acid gas adopts liquid amine, and its main component is diethanolamine that can be water-soluble.Although this alkanolamine solution is prepared fairly simple, there is many shortcomings in it: the first, and this performance of the adsorbent is poor, and adsorption efficiency is low.The second, the weight of liquid amine sorbent material is large.3rd, at adsorption/desorption CO
2process in have the loss of amine, make reprocessing cycle efficiency low, secondary pollution caused to environment.
Summary of the invention
The technical problem that the present invention mainly solves: in carbon dioxide treatment process, physisorphtion and chemiadsorption adsorption poor, adsorption efficiency is low, and chemosorbent can cause secondary pollution and the inefficient problem of reprocessing cycle to environment, provide one to carbonize with safety tree root stem, as charcoal base, then to be oxidized two niobiums, the materials such as zirconium diboride are as raw material, make ceramic matrix, subsequently charcoal base is mixed with ceramic matrix, under acidic conditions and catalyst action, preliminary modification, last under argon atmosphere, high-temperature calcination, and quench, expand the space of matrix material, and modification internal structure, thus the method obtained for absorbing carbon dioxide ceramic composite.Absorbing carbon dioxide ceramic composite absorption property prepared by the present invention is good, and adsorption efficiency improves 10 ~ 15%, can recycled for multiple times, can not cause secondary pollution to environment.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention:
(1) get 800 ~ 900g safety tree root stem, use water to be cleaned on its surface, then put it in baking oven, at temperature is 70 ~ 80 DEG C, dry, put it in extrusion machine subsequently, block is squeezed under 1 ~ 3MPa, the block of gained is put into smokeless charring furnace, at temperature is 200 ~ 240 DEG C, charing 30 ~ 40min, after charing terminates, charing safety tree root stem is put into pulverizer pulverize, sieve to obtain 180 ~ 200 order charing powder, for subsequent use;
(2) count by weight, get 20 ~ 30 parts of titanium dioxide, 10 ~ 15 parts of Niobium Pentxoxides, 10 ~ 20 parts of zirconium diborides, 30 ~ 35 parts of polydimethylsiloxane and 10 ~ 20 parts of aluminum oxide, after mixing, put it in high-temperature calcination stove, use nitrogen protection, at temperature is 1000 ~ 1200 DEG C, after calcining 2 ~ 3h, taken out, be down to room temperature, then put it in ball mill and grind, sieve to obtain 200 ~ 220 order ceramic matrixs;
(3) count by weight, get the ceramic matrix of 55 ~ 65 parts of above-mentioned gained, the charing powder of 25 ~ 30 parts of step (1) gained, 5 ~ 10 parts of massfractions are 30% Platinic chloride and 3 ~ 7 parts of palladous oxides, mix, then put it in container, subsequently container is moved in ultrasonator, under frequency 80 ~ 120KHz, vibration 50 ~ 70min;
(4) after above-mentioned vibration terminates, container is moved in calcining furnace, argon gas is filled with in calcining furnace, the flow rate set of argon gas is 2 ~ 5mL/min, then with the heat-up rate of 10 ~ 15 DEG C/min, is warming up to 600 ~ 800 DEG C, keep temperature 10 ~ 20min, subsequently with the heat-up rate of 4 ~ 6 DEG C/min, after being warming up to 1200 ~ 1300 DEG C, keep temperature 50 ~ 70min;
(5) after above-mentioned insulation terminates, stop heating, then cool to 300 ~ 400 DEG C with the furnace, then is taken out and to move in quenching machine quenching 10 ~ 15min, taken out subsequently and be cooled to room temperature, can obtain for absorbing carbon dioxide ceramic composite.
Prepared by the present invention is 300 ~ 450m for absorbing carbon dioxide ceramic composite specific surface area
2/ g, pore volume is 0.05 ~ 0.2cc/g.
application of the present invention: the absorbing carbon dioxide ceramic composite that is used for of above-mentioned preparation is placed in vacuum drying box, vacuum is filled at constant temperature 120 ~ 130 DEG C, after drying 1 ~ 2h, carbonic acid gas is passed into it, controlling it, to pass into flow be 100 ~ 120mL/min, its adsorption time is made to be 30 ~ 40min, take out sorbent material, be placed in electronic-weighing, can find that adsorption efficiency reaches more than 99%, prepared by the present invention can be used for the industry such as fossil fuel power, production for absorbing carbon dioxide ceramic composite.
The invention has the beneficial effects as follows:
(1) the absorbing carbon dioxide ceramic composite absorption property prepared is good, and adsorption efficiency improves 10 ~ 15%;
(2) can recycled for multiple times, secondary pollution can not be caused to environment;
(3) preparation process is simple, and cost is low.
Embodiment
First get 800 ~ 900g safety tree root stem, use water to be cleaned on its surface, then put it in baking oven, at temperature is 70 ~ 80 DEG C, dry, put it in extrusion machine subsequently, block is squeezed under 1 ~ 3MPa, the block of gained is put into smokeless charring furnace, at temperature is 200 ~ 240 DEG C, charing 30 ~ 40min, after charing terminates, charing safety tree root stem is put into pulverizer pulverize, sieve to obtain 180 ~ 200 order charing powder, for subsequent use; Count by weight again, get 20 ~ 30 parts of titanium dioxide, 10 ~ 15 parts of Niobium Pentxoxides, 10 ~ 20 parts of zirconium diborides, 30 ~ 35 parts of polydimethylsiloxane and 10 ~ 20 parts of aluminum oxide, after mixing, put it in high-temperature calcination stove, use nitrogen protection, at temperature is 1000 ~ 1200 DEG C, after calcining 2 ~ 3h, taken out, be down to room temperature, then put it in ball mill and grind, sieve to obtain 200 ~ 220 order ceramic matrixs; Count by weight, get the ceramic matrix of 55 ~ 65 parts of above-mentioned gained, 25 ~ 30 parts of charing powder, 5 ~ 10 parts of massfractions are 30% Platinic chloride and 3 ~ 7 parts of palladous oxides, mix, then put it in container, subsequently container is moved in ultrasonator, under frequency 80 ~ 120KHz, vibration 50 ~ 70min; After above-mentioned vibration terminates, container is moved in calcining furnace, argon gas is filled with in calcining furnace, the flow rate set of argon gas is 2 ~ 5mL/min, then with the heat-up rate of 10 ~ 15 DEG C/min, is warming up to 600 ~ 800 DEG C, keep temperature 10 ~ 20min, subsequently with the heat-up rate of 4 ~ 6 DEG C/min, after being warming up to 1200 ~ 1300 DEG C, keep temperature 50 ~ 70min; After above-mentioned insulation terminates, stop heating, then cool to 300 ~ 400 DEG C with the furnace, then is taken out and to move in quenching machine quenching 10 ~ 15min, taken out subsequently and be cooled to room temperature, can obtain for absorbing carbon dioxide ceramic composite.
Example 1
First get 900g safety tree root stem, use water to be cleaned on its surface, then put it in baking oven, at temperature is 80 DEG C, dry, put it in extrusion machine subsequently, block is squeezed under 3MPa, the block of gained is put into smokeless charring furnace, at temperature is 240 DEG C, charing 40min, after charing terminates, charing safety tree root stem is put into pulverizer pulverize, sieve to obtain 200 order charing powder, for subsequent use; Count by weight again, get 25 parts of titanium dioxide, 10 parts of Niobium Pentxoxides, 10 parts of zirconium diborides, 35 parts of polydimethylsiloxane and 20 parts of aluminum oxide, after mixing, put it in high-temperature calcination stove, use nitrogen protection, at temperature is 1200 DEG C, after calcining 3h, taken out, be down to room temperature, then put it in ball mill and grind, sieve to obtain 220 order ceramic matrixs; Count by weight, get the ceramic matrix of 65 parts of above-mentioned gained, 25 parts of charing powder, 5 parts of massfractions are 30% Platinic chloride and 5 parts of palladous oxides, mix, then put it in container, subsequently container is moved in ultrasonator, under frequency 100KHz, vibration 70min; After above-mentioned vibration terminates, container is moved in calcining furnace, argon gas is filled with in calcining furnace, the flow rate set of argon gas is 5mL/min, then with the heat-up rate of 15 DEG C/min, is warming up to 800 DEG C, keep temperature 20min, subsequently with the heat-up rate of 6 DEG C/min, after being warming up to 1300 DEG C, keep temperature 70min; After above-mentioned insulation terminates, stop heating, then cool to 400 DEG C with the furnace, then taken out and move in quenching machine the 15min that quenches, taken out subsequently and be cooled to room temperature, can obtain for absorbing carbon dioxide ceramic composite.The absorbing carbon dioxide ceramic composite that is used for of above-mentioned preparation is placed in vacuum drying box, vacuum is filled at constant temperature 130 DEG C, after drying 2h, carbonic acid gas is passed into it, controlling it, to pass into flow be 120mL/min, makes its adsorption time be 40min, takes out sorbent material, be placed in electronic-weighing, can find that adsorption efficiency reaches 99.2%.
example 2
First get 800g safety tree root stem, use water to be cleaned on its surface, then put it in baking oven, at temperature is 70 DEG C, dry, put it in extrusion machine subsequently, block is squeezed under 1MPa, the block of gained is put into smokeless charring furnace, at temperature is 200 DEG C, charing 30min, after charing terminates, charing safety tree root stem is put into pulverizer pulverize, sieve to obtain 180 order charing powder, for subsequent use; Count by weight again, get 20 parts of titanium dioxide, 15 parts of Niobium Pentxoxides, 20 parts of zirconium diborides, 35 parts of polydimethylsiloxane and 10 parts of aluminum oxide, after mixing, put it in high-temperature calcination stove, use nitrogen protection, at temperature is 1200 DEG C, after calcining 3h, taken out, be down to room temperature, then put it in ball mill and grind, sieve to obtain 220 order ceramic matrixs; Count by weight, get the ceramic matrix of 55 parts of above-mentioned gained, 30 parts of charing powder, 10 parts of massfractions are 30% Platinic chloride and 5 parts of palladous oxides, mix, then put it in container, subsequently container is moved in ultrasonator, under frequency 80KHz, vibration 50min; After above-mentioned vibration terminates, container is moved in calcining furnace, argon gas is filled with in calcining furnace, the flow rate set of argon gas is 2mL/min, then with the heat-up rate of 10 DEG C/min, is warming up to 600 DEG C, keep temperature 10min, subsequently with the heat-up rate of 4 DEG C/min, after being warming up to 1200 DEG C, keep temperature 50min; After above-mentioned insulation terminates, stop heating, then cool to 300 DEG C with the furnace, then taken out and move in quenching machine the 10min that quenches, taken out subsequently and be cooled to room temperature, can obtain for absorbing carbon dioxide ceramic composite.The absorbing carbon dioxide ceramic composite that is used for of above-mentioned preparation is placed in vacuum drying box, vacuum is filled at constant temperature 120 DEG C, after drying 1h, carbonic acid gas is passed into it, controlling it, to pass into flow be 100mL/min, makes its adsorption time be 30min, takes out sorbent material, be placed in electronic-weighing, can find that adsorption efficiency reaches 99.6%.
Example 3
First get 850g safety tree root stem, use water to be cleaned on its surface, then put it in baking oven, at temperature is 75 DEG C, dry, put it in extrusion machine subsequently, block is squeezed under 2MPa, the block of gained is put into smokeless charring furnace, at temperature is 220 DEG C, charing 32min, after charing terminates, charing safety tree root stem is put into pulverizer pulverize, sieve to obtain 190 order charing powder, for subsequent use; Count by weight again, get 25 parts of titanium dioxide, 15 parts of Niobium Pentxoxides, 20 parts of zirconium diborides, 30 parts of polydimethylsiloxane and 10 parts of aluminum oxide, after mixing, put it in high-temperature calcination stove, use nitrogen protection, at temperature is 1100 DEG C, after calcining 2h, taken out, be down to room temperature, then put it in ball mill and grind, sieve to obtain 210 order ceramic matrixs; Count by weight, get the ceramic matrix of 60 parts of above-mentioned gained, 25 parts of charing powder, 10 parts of massfractions are 30% Platinic chloride and 5 parts of palladous oxides, mix, then put it in container, subsequently container is moved in ultrasonator, under frequency 100KHz, vibration 60min; After above-mentioned vibration terminates, container is moved in calcining furnace, argon gas is filled with in calcining furnace, the flow rate set of argon gas is 3mL/min, then with the heat-up rate of 12 DEG C/min, is warming up to 700 DEG C, keep temperature 15min, subsequently with the heat-up rate of 5 DEG C/min, after being warming up to 1250 DEG C, keep temperature 60min; After above-mentioned insulation terminates, stop heating, then cool to 350 DEG C with the furnace, then taken out and move in quenching machine the 12min that quenches, taken out subsequently and be cooled to room temperature, can obtain for absorbing carbon dioxide ceramic composite.The absorbing carbon dioxide ceramic composite that is used for of above-mentioned preparation is placed in vacuum drying box, vacuum is filled at constant temperature 125 DEG C, after drying 1h, carbonic acid gas is passed into it, controlling it, to pass into flow be 110mL/min, makes its adsorption time be 35min, takes out sorbent material, be placed in electronic-weighing, can find that adsorption efficiency reaches 99.5%.
Claims (1)
1., for a preparation method for absorbing carbon dioxide ceramic composite, it is characterized in that concrete preparation process is:
(1) get 800 ~ 900g safety tree root stem, use water to be cleaned on its surface, then put it in baking oven, at temperature is 70 ~ 80 DEG C, dry, put it in extrusion machine subsequently, block is squeezed under 1 ~ 3MPa, the block of gained is put into smokeless charring furnace, at temperature is 200 ~ 240 DEG C, charing 30 ~ 40min, after charing terminates, charing safety tree root stem is put into pulverizer pulverize, sieve to obtain 180 ~ 200 order charing powder, for subsequent use;
(2) count by weight, get 20 ~ 30 parts of titanium dioxide, 10 ~ 15 parts of Niobium Pentxoxides, 10 ~ 20 parts of zirconium diborides, 30 ~ 35 parts of polydimethylsiloxane and 10 ~ 20 parts of aluminum oxide, after mixing, put it in high-temperature calcination stove, use nitrogen protection, at temperature is 1000 ~ 1200 DEG C, after calcining 2 ~ 3h, taken out, be down to room temperature, then put it in ball mill and grind, sieve to obtain 200 ~ 220 order ceramic matrixs;
(3) count by weight, get the ceramic matrix of 55 ~ 65 parts of above-mentioned gained, the charing powder of 25 ~ 30 parts of step (1) gained, 5 ~ 10 parts of massfractions are 30% Platinic chloride and 3 ~ 7 parts of palladous oxides, mix, then put it in container, subsequently container is moved in ultrasonator, under frequency 80 ~ 120KHz, vibration 50 ~ 70min;
(4) after above-mentioned vibration terminates, container is moved in calcining furnace, argon gas is filled with in calcining furnace, the flow rate set of argon gas is 2 ~ 5mL/min, then with the heat-up rate of 10 ~ 15 DEG C/min, is warming up to 600 ~ 800 DEG C, keep temperature 10 ~ 20min, subsequently with the heat-up rate of 4 ~ 6 DEG C/min, after being warming up to 1200 ~ 1300 DEG C, keep temperature 50 ~ 70min;
(5) after above-mentioned insulation terminates, stop heating, then cool to 300 ~ 400 DEG C with the furnace, then is taken out and to move in quenching machine quenching 10 ~ 15min, taken out subsequently and be cooled to room temperature, can obtain for absorbing carbon dioxide ceramic composite.
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| CN103566881A (en) * | 2013-09-29 | 2014-02-12 | 安徽金叶炭素科技有限公司 | Modified activated carbon of plant roots and preparation method thereof |
| CN103691200A (en) * | 2014-01-13 | 2014-04-02 | 魏耘 | Air filtering medium material, medium, filter and air filtering method |
| CN104743556A (en) * | 2015-03-26 | 2015-07-01 | 中国科学院生态环境研究中心 | Powder active carbon prepared by using turf as raw material and preparation method of powder active carbon |
| CN104961340A (en) * | 2015-06-10 | 2015-10-07 | 安徽省德邦瓷业有限公司 | Weatherproof and durable glass ceramic disc and preparation method thereof |
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