CN103933935B - A kind of method improving active carbon carbon dioxide adsorption performance - Google Patents
A kind of method improving active carbon carbon dioxide adsorption performance Download PDFInfo
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- CN103933935B CN103933935B CN201410132974.5A CN201410132974A CN103933935B CN 103933935 B CN103933935 B CN 103933935B CN 201410132974 A CN201410132974 A CN 201410132974A CN 103933935 B CN103933935 B CN 103933935B
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Abstract
The invention discloses a kind of method improving active carbon carbon dioxide adsorption performance, impregnation technology improvement is adopted to active carbon similar to molecular sieve, maceration extract is made up of the potassium sulfate solution of 1-3mol/L and the ammonium persulfate solution of 0.5mol/L, maceration extract and active carbon are fully mixed to bubble-free, then be heated to 50-70 DEG C, be incubated to solution complete reaction until disappear, then use distilled water detergent active charcoal, at 120-150 DEG C, be dried to constant weight after having washed, obtain activated carbon product.The activated carbon product that the present invention obtains, can make active carbon to the adsorbance of carbon dioxide, original basis increases 20-40%.Active carbon carbon dioxide adsorption testing arrangement and method are shown in accompanying drawing.The activated carbon product that the present invention obtains, has the advantages that Gas Phase Adsorption is effective, for the process for purifying of high-purity gas, can increase substantially operating efficiency.
Description
Technical field
The present invention relates to a kind of technology improving active carbon carbon dioxide adsorption performance, especially relate to the ameliorative way that a kind of raw material active carbon is the carbon dioxide adsorption performance of the active carbon of quasi-molecule sieve-type structure.
Background technology
Active carbon similar to molecular sieve product has special micropore distribution, and micropore prosperity high concentration again, is mainly used on high-purity gas process for purifying.Refine the active carbon similar to molecular sieve product of being used widely in hydrogen field at petroleum chemical industry pressure-variable adsorption, be mainly used in Adsorption carbon dioxide impurities gas, therefore, the carbon dioxide adsorption performance quality of active carbon is very crucial.Research shows, the aperture structure of active carbon and surface nature are the principal elements affecting its carbon dioxide adsorption performance.
Summary of the invention
The invention provides a kind of technology improving active carbon carbon dioxide adsorption performance, especially relate to the ameliorative way that a kind of raw material active carbon is the carbon dioxide adsorption performance of the active carbon of quasi-molecule sieve-type structure.Be adopt impregnation technology, improved the carbon dioxide adsorption performance of active carbon by the method changing activated carbon surface functional group character.The activated carbon product obtained by the present invention has the effective advantage of carbon dioxide adsorption, can be used for the process for purifying of high-purity gas, improves gas purification efficiency.
The present invention adopts following technical scheme to be: a kind of method improving active carbon carbon dioxide adsorption performance, impregnation technology improvement is adopted to active carbon similar to molecular sieve, maceration extract is made up of the potassium sulfate solution of 1-3mol/L and the ammonium persulfate solution of 0.5mol/L, maceration extract and active carbon are fully mixed to bubble-free, then 50-70 DEG C is heated to, insulation is to solution complete reaction until disappear, use distilled water detergent active charcoal again, at 120-150 DEG C, be dried to constant weight after having washed, obtain activated carbon product.
The 1:1 mixing by volume of potassium sulfate solution and ammonium persulfate solution, carries out impregnation process in the ratio adding 50 grams of active carbons in every 50ml-100ml maceration extract.
Maceration extract is made up of the potassium sulfate solution of 1mol/L and the ammonium persulfate solution of 0.5mol/L, in the ratio mixing adding 50 grams of active carbons in every 50ml-100ml maceration extract.
Described active carbon similar to molecular sieve is ature of coal or coconut husk active carbon similar to molecular sieve.
Described active carbon similar to molecular sieve, wherein radius is less than
pore volume account for total pore volume be greater than 90%, by BET computational methods specific area at 800m
2/ g-1150m
2/ g, probe temperature 25 DEG C, test gas pressure 0.1MPa(absolute pressure), vacuum of finding time-0.093MPa(gauge pressure) condition under, carbon dioxide adsorption index is at more than 50ml/g, and the scuff resistance of product is more than 98%.
Beneficial effect:
1, the technology of the present invention is shaped at active carbon similar to molecular sieve pore structure, its carbon dioxide adsorption has been on the basis of definite value, adopt impregnation technology, have selected especially and be made up of (potassium sulfate solution: ammonium persulfate solution=1:1(volume) the potassium sulfate solution of 1-3mol/L and the ammonium persulfate solution of 0.5mol/L) maceration extract process active carbon similar to molecular sieve raw material, remarkable change activated carbon surface functional group character, the carbon dioxide adsorption performance of active carbon is improved further by the method changing activated carbon surface character, on original basis, the carbon dioxide adsorption of active carbon increases 20-40%.Product is used for the process for purifying of high-purity gas, can significantly improve gas purification efficiency further.For same adsorbent equipment, the use amount of active carbon can be reduced and improve the purity of product gas, thus bringing significant economic benefit.
2, technology of the present invention is applicable to all types of for the active carbon similar to molecular sieve based on absorbing carbon dioxide.Described active carbon similar to molecular sieve, wherein radius is less than
pore volume account for total pore volume be greater than 90%, by BET computational methods specific area at 800m
2/ g-1150m
2/ g, probe temperature 25 DEG C, test gas pressure 0.1MPa(absolute pressure), vacuum of finding time-0.093MPa(gauge pressure) condition under, carbon dioxide adsorption index is at more than 50ml/g, and the scuff resistance of product is more than 98%.Modified through flooding, hydroxyl and the carboxyl functional group of activated carbon surface significantly increase, and original pore structure can not change (aperture structure that activating process determines active carbon), modified active carbon carbon dioxide adsorption improves more than 20%, reaches more than 60ml/g.
3, the present invention adopt potassium sulfate and ammonium persulfate mixed impregnant liquor, to production equipment without any corrosion, essentially no environmental pollution.
Accompanying drawing explanation
The carbon dioxide adsorption testing arrangement figure of Fig. 1 active carbon.
1-carbon dioxide air source, 2-pressure gauge, 3-silica dehydrator bottle, 4-spinner flowmeter, 5-coiled pipe, 6-adsorption tube, 7-thermostatical water bath, 8-gas buffer bottle, 9-vacuum meter, 10-vavuum pump, K1 ~ K5 are cock.
The infrared spectrum of Fig. 2 active carbon.
Detailed description of the invention
The carbon dioxide adsorption testing arrangement of active carbon of the present invention is for shown in Fig. 1, and active carbon carbon dioxide adsorption method of testing is:
Active carbon sample is dried to constant weight at 110 ± 5 DEG C, be placed in drier for subsequent use, adsorption tube being cleaned rear weighing is that m1 is (together with pipe close, be accurate to 1mg), ready sample is divided two to three times load in adsorption tube, layer of charcoal is high, and (10 ± 0.2) ㎝ (height after jolt ramming), after filling, pipe close is coated vaseline spin, weigh together with pipe close and weigh again as m2(is accurate to 1mg).Weigh complete, adsorption tube is vertically inserted (bath temperature 25 DEG C) in water bath with thermostatic control.
After everything in readiness, first with high-purity helium purge adsorbent, after finding time, pass into high-purity carbon dioxide gas to be measured, vacuum of finding time-0.093Mpa (gauge pressure).Then cock K1, K2 is opened, cut-out tap K3, connect carbon dioxide steel cylinder source of the gas, regulate K1, until steady air current is at (1670 ± 70) ml/min flow, then cock K3, K4 is opened, cut-out tap K2, K5, make air-flow by sample 1 hour, then open K2, close K3, it is that m3(is accurate to 1mg that taking-up adsorption tube cleans rear weighing).By in adsorption tube again embedding device, open K3, close K2, make sample again by sample 10 minutes, repeat aforesaid operations, till adsorbing saturated (the of poor quality of twice weighing is not more than 10mg).Then source of the gas is closed, off-test.
Active carbon is to the adsorbance of carbon dioxide:
Q=509.1（m3-m2）/（m2-m1）×100%
In formula:
The quality of m1-adsorption tube, g;
Before m2-absorption, adsorption tube adds the quality of charcoal, g;
After m3-absorption, adsorption tube adds the quality of charcoal and carbon dioxide, g;
Q-active carbon to the adsorbance (1atm, 25 DEG C) of carbon dioxide, ml/g.
Embodiment 1.
1, improving a method for active carbon carbon dioxide adsorption performance, is when active carbon similar to molecular sieve pore structure is shaped, and adopts impregnation technology, is improved the carbon dioxide adsorption performance of active carbon by the method changing activated carbon surface character.Maceration extract is made up of (potassium sulfate solution: ammonium persulfate solution=1:1(volume ratio) the potassium sulfate solution of 1-3mol/L and the ammonium persulfate solution of 0.5mol/L).In the ratio adding 50 grams of active carbons in 50ml maceration extract, be fully mixed to bubble-free, be then heated to 50-70 DEG C, be incubated to solution complete reaction until disappear, then use distilled water detergent active charcoal, until the pH value of cleaning fluid and distilled water is basically identical.At 120-150 DEG C, be dried to constant weight after having washed, namely can be made into topic and state activated carbon product.The activated carbon product that the present invention obtains, can make active carbon to the adsorbance of carbon dioxide, original basis increases 20-40%.
On employing market, common ature of coal and coconut husk active carbon similar to molecular sieve are as sample, and infrared spectrum is shown in that (H900 represents ature of coal active carbon similar to molecular sieve to Fig. 2, and C900 represents coconut husk active carbon similar to molecular sieve.
As can be seen from the figure, the surface characteristics absworption peak of two species sieve-type active carbons is basically identical, at 3400cm
-1place is O-H stretching vibration characteristic peak, 2800cm
-1place is saturated C-H characteristic peak, 1600cm
-1place is C=O stretching vibration characteristic peak, 1450cm
-1place is O-H flexural vibrations, 1150cm
-1place is the stretching vibration peak of C-O, it can thus be appreciated that activated carbon surface functional group mainly contains hydroxyl, carbonyl and carboxyl etc.
Ature of coal common on market and coconut husk active carbon similar to molecular sieve through the modified absorption property of the embodiment of the present invention 1 and surface functional group number change situation as shown in table 1, wherein MZ represents coal mass active carbon, and YK represents cocoanut active charcoal.
The concentration of the activated carbon modified front and rear surfaces functional group of table 1 and CO
2adsorption capacity
Note: by Beohm titration measuring active carbon and modified surface functional group concentration.Beohm titration is the oxy radical generation acid-base neutralization reaction different from activated carbon surface according to different alkali, it is generally acknowledged, NaHCO3 can carboxylic acid group in Neutralization effect carbon surface functional group, with carboxylic acid group and lactones base in Na2CO3, in NaOH and phenolic hydroxyl group, lactones base and carboxylic acid group, C2H5ONa can in and phenolic hydroxyl group, lactones base, carboxylic acid group and carbonyl.
Embodiment 2.
Improve a method for active carbon carbon dioxide adsorption performance, be adopt impregnation technology, improved the carbon dioxide adsorption performance of active carbon by the method changing activated carbon surface character.Maceration extract is made up of (potassium sulfate solution: ammonium persulfate solution=1:1(volume ratio) the potassium sulfate solution of 1mol/L and the ammonium persulfate solution of 0.5mol/L).In the ratio adding 50 grams of active carbons in 60ml maceration extract, be fully mixed to bubble-free, be then heated to 50 DEG C, be incubated to solution complete reaction until disappear, then use distilled water detergent active charcoal, until the pH value of cleaning fluid and distilled water is basically identical.At 120 DEG C, be dried to constant weight after having washed, namely can be made into topic and state activated carbon product.The activated carbon product that the present invention obtains, can make active carbon to the adsorbance of carbon dioxide, and original basis increases by 20%.
Embodiment 3.
Improve a method for active carbon carbon dioxide adsorption performance, be adopt impregnation technology, improved the carbon dioxide adsorption performance of active carbon by the method changing activated carbon surface character.Maceration extract is made up of (potassium sulfate solution: ammonium persulfate solution=1:1(volume) the potassium sulfate solution of 2mol/L and the ammonium persulfate solution of 0.5mol/L).In the ratio adding 50 grams of active carbons in 70ml maceration extract, be fully mixed to bubble-free, be then heated to 60 DEG C, be incubated to solution complete reaction until disappear, then use distilled water detergent active charcoal, until the pH value of cleaning fluid and distilled water is basically identical.At 130 DEG C, be dried to constant weight after having washed, namely can be made into topic and state activated carbon product.The activated carbon product that the present invention obtains, can make active carbon to the adsorbance of carbon dioxide, and original basis increases by 30%.
Embodiment 4.
Improve a method for active carbon carbon dioxide adsorption performance, be adopt impregnation technology, improved the carbon dioxide adsorption performance of active carbon by the method changing activated carbon surface character.Maceration extract is made up of (potassium sulfate solution: ammonium persulfate solution=1:1(volume) the potassium sulfate solution of 3mol/L and the ammonium persulfate solution of 0.5mol/L).In the ratio adding 50 grams of active carbons in 90ml maceration extract, be fully mixed to bubble-free, be then heated to 70 DEG C, be incubated to solution complete reaction until disappear, then use distilled water detergent active charcoal, until the pH value of cleaning fluid and distilled water is basically identical.At 150 DEG C, be dried to constant weight after having washed, namely can be made into topic and state activated carbon product.The activated carbon product that the present invention obtains, can make active carbon to the adsorbance of carbon dioxide, and original basis increases by 40%.
Embodiment 5
Improve a method for active carbon carbon dioxide adsorption performance, be adopt impregnation technology, improved the carbon dioxide adsorption performance of active carbon by the method changing activated carbon surface character.Maceration extract is made up of (potassium sulfate solution: ammonium persulfate solution=1:1(volume) the potassium sulfate solution of 2mol/L and the ammonium persulfate solution of 0.5mol/L).In the ratio adding 50 grams of active carbons in 100ml maceration extract, be fully mixed to bubble-free, be then heated to 60 DEG C, be incubated to solution complete reaction until disappear, then use distilled water detergent active charcoal, until the pH value of cleaning fluid and distilled water is basically identical.At 130 DEG C, be dried to constant weight after having washed, namely can be made into topic and state activated carbon product.
Claims (4)
1. one kind is improved the method for active carbon carbon dioxide adsorption performance, it is characterized in that, impregnation technology improvement is adopted to active carbon similar to molecular sieve, maceration extract is made up of the potassium sulfate solution of 1mol/L and the ammonium persulfate solution of 0.5mol/L, in the ratio mixing adding 50 grams of active carbons in every 50ml-100ml maceration extract, maceration extract and active carbon are fully mixed to bubble-free, then 50-70 DEG C is heated to, insulation is to solution complete reaction until disappear, use distilled water detergent active charcoal again, at 120-150 DEG C, be dried to constant weight after having washed, obtain activated carbon product.
2. improve the method for active carbon carbon dioxide adsorption performance as claimed in claim 1, it is characterized in that, the 1:1 mixing by volume of potassium sulfate solution and ammonium persulfate solution, carries out impregnation process in the ratio adding 50 grams of active carbons in every 50mL-100mL maceration extract.
3. improve the method for active carbon carbon dioxide adsorption performance as claimed in claim 1, it is characterized in that, described active carbon similar to molecular sieve is ature of coal or coconut husk active carbon similar to molecular sieve.
4. improve the method for active carbon carbon dioxide adsorption performance as claimed in claim 1, it is characterized in that, described active carbon similar to molecular sieve, what the pore volume that wherein radius is less than 9 accounted for total pore volume is greater than 90%, by BET computational methods specific area at 800m
2/ g-1150m
2/ g, probe temperature 25 DEG C, test gas pressure, under the condition of vacuum of finding time-0.093MPa gauge pressure, carbon dioxide adsorption index is at more than 50ml/g, and the scuff resistance of product is more than 98%.
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