CN105381791A - Preparation method of attapulgite-based molecular imprinting type CO2 adsorbing material - Google Patents
Preparation method of attapulgite-based molecular imprinting type CO2 adsorbing material Download PDFInfo
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- CN105381791A CN105381791A CN201510803546.5A CN201510803546A CN105381791A CN 105381791 A CN105381791 A CN 105381791A CN 201510803546 A CN201510803546 A CN 201510803546A CN 105381791 A CN105381791 A CN 105381791A
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- molecular imprinting
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- attapulgite clay
- sorbing material
- soil matrix
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Abstract
The invention discloses a preparation method of an attapulgite-based molecular imprinting type CO2 adsorbing material. The method comprises: reacting by using a silane coupling agent and attapulgite clay to obtain modified attapulgite clay; soaking an initiator, a cross-linking agent, a monomer and a template in hole channels of the modified attapulgite clay, triggering polymerization, and generating cross-linked polymers in hole channels of the modified attapulgite clay through triggering polymerization; and eluting the template by using an elution solvent to obtain the attapulgite-based molecular imprinting type CO2 adsorbing material having amino functional groups. The preparation method disclosed by the invention is simple, easy to operate and liable in industrial production; a prepared adsorbent can be repeatedly used, is high in adsorptive selectivity on CO2, and is wide in application prospect.
Description
Technical field
The present invention relates to the preparation method of attapulgite clay adsorbent, be specifically related to a kind of CO
2adsorb the preparation method with recessed soil matrix molecular imprinting sorbing material.
Background technology
CO
2be one of main greenhouse gases, through the shortwave radiation of the sun, the long-wave radiation of the earth can be absorbed, thus the temperature of earth's surface or inferior atmospheric layer is raised, cause " greenhouse effects ".Since the industrial revolution, because the mankind too rely on fossil energy, cause the CO in air
2concentration constantly increases.2013, CO
2discharge capacity reaches record-breaking 36,000,000,000 tons, considerably beyond the CO that photosynthesis of plant consumes
2amount.Fossil fuel is most important part in present stage world energy sources structure, and the alternative energy source developing new cheapness also needs a period of time grown very much.In this case, to the CO produced
2carrying out trapping recovery is the most direct, effective carbon emission reduction means.At present, to CO
2the method that trapping is reclaimed mainly contains absorption process, low temperature processing, membrane separation process and absorption method etc., and wherein absorption method has the advantages such as energy consumption is low, adsorbance is large, equipment is simple, easy to operate, selective height, applied range, is competitive a kind of CO
2recovery technology.And the selection of sorbing material and development are absorption method separation of C O
2one of key factor of technology.
Attapulgite clay (ATP, recessed soil), also known as palygorskite, belongs to rare nonmetallic ore class.In the Luhe of Su-Wan area, little winding, the ground such as Mingguang, anhui and Xuyi Jiangsu has found that reserves are concentrated, cheap, has easily exploited in China, has important industrial application value.Owing to having regular layer chain structure and larger specific area and pore volume, and the siliceous hydroxyl activity site of rich surface, be easy to introduce functional group on surface, therefore, recessed soil can as a kind of good adsorbent, as a kind of adsorbing agent carrier of cheapness, alkaline density and adsorption activity position can be improved by surface modifying method, thus be applied to CO
2separation.At present, also fewer for the research report of gas absorption about attapulgite clay.
Summary of the invention
The object of the invention is: a kind of recessed soil matrix molecular imprinting CO is provided
2the preparation method of sorbing material, this CO
2the adsorption capacity of sorbing material is large, by force selective.
Technical solution of the present invention is: adopt silane coupler and attapulgite clay to react, carry out surface-functionalized, obtained modified attapulgite clay; Then initator, crosslinking agent, monomer and template are immersed in the duct of modified attapulgite clay, by initiated polymerization, in attapulgite clay duct, generate cross-linked polymer; Finally use eluting solvent eluted template, obtain the recessed soil matrix molecular imprinting sorbing material with amidine functional group; Its concrete operation step is as follows:
First step: by attapulgite clay 105 DEG C oven dry, pulverized 200 orders; Add attapulgite clay and the 100-150 weight parts organic solvent of 3 weight portions oven dry in a reservoir, in whipping process, add 3-5 weight portion silane coupler, in 40-45 DEG C of ultrasonic wave, react 30-50 minute; 3-5 hour is reacted again in the constant temperature oil bath of 40-60 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
Second step: the function monomer of 2-8mmol and 1mmol template molecule are placed in reactor, add 10-20mmol solvent, sealing, ultrasonic disperse 10-20 minute, makes whole system fully dissolve and mixes; This system is left standstill 12-24 hour at room temperature condition, template molecule and function monomer is fully acted on, forms stable compound;
Third step: add 10-30mmol crosslinking agent, 0.3-0.5mol initator and 1-2g modified attapulgite clay in the template molecule-function monomer complex systems of above-mentioned step 2, ultrasonic degas 10-20 minute, lead to after air all being replaced in inert gas 10-20 minute again, reactor is sealed, 50-80 DEG C of constant temperature initiated polymerization 24-48 hour;
4th step: step 3 polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with eluting solvent cyclic washing 24-36 hour, template molecule in removing product and other unreacted reactant, till can't detect the template in eluent with ultraviolet-uisible spectrophotometer, then with high purity water washing, 105 DEG C of dryings, obtain CO
2molecular imprinting absorbent.
Wherein, the coupling agent of employing is silane coupler: γ-(methacryloxypropyl) propyl trimethoxy silicane, APTES.
Wherein, the organic solvent adopted in first step is toluene or absolute ethyl alcohol.
Wherein, the template molecule of employing is acetic acid or ethanedioic acid.
Wherein, the function monomer of employing is acrylamide.
Wherein, the solvent that second step adopts is: acetonitrile, toluene, or the mixed solvent of acetonitrile and toluene; Wherein acetonitrile: the volume ratio of toluene is 1:1.
Wherein, the crosslinking agent of employing is ethylene glycol dimethacrylate (EGDMA), N, N '-methylene-bisacrylamide.
Wherein, the initator of employing is that azo-initiator is as azodiisobutyronitrile.
Wherein, inert gas is nitrogen.
Wherein, the eluting solvent adopted in the 4th step is: methyl alcohol, the mixed solvent of hydrochloric acid and methyl alcohol; Its hydrochloric acid: the volume ratio of methyl alcohol is 1:9.
the present invention has the following advantages:
(1) the recessed soil matrix molecular imprinting polymer that obtains of the present invention, is added with template molecule in building-up process, by the means removing of template molecule by physics or chemistry after being polymerized, thus stays CO in recessed native duct
2there is the hole of selective absorption effect, this adsorbent cavity surface contain can with CO
2there is amino-functional group that is strong and effect in molecule, thus substantially increases absorption property and adsorptive selectivity.
(2) present invention uses cheap attapulgite clay, the cost of compound adsorbent is reduced greatly, and this adsorbent has larger adsorption capacity and adsorptive selectivity, and aperture structure is even, and specific area is comparatively large, and size tunable system, regeneration energy consumption is low.
(3) adsorbent of the present invention is highly cross-linked polymer, and its compression strength and stability better, are suitable for use as the CO produced in suitability for industrialized production
2adsorbent, for minimizing CO
2discharge, slow down Global Greenhouse Effect there is very strong realistic meaning.
(4) compound adsorbent preparation method is simple, and easy to operate, be easy to suitability for industrialized production, reagent used is conventional reagent, and equipment is basic equipment, and preparation cost is low.
(5) this adsorbent can repeatedly use, and can not cause secondary pollution to environment.
Accompanying drawing explanation
Fig. 1 is recessed soil matrix molecular imprinting CO
2sorbing material prepare schematic diagram;
Fig. 2 is homemade adsorption experimental apparatus flow chart;
Fig. 3 is the infrared spectrum of recessed soil, coupling agent modified recessed soil, recessed soil matrix molecular imprinting sorbing material and the non-molecular engram sorbing material of recessed soil matrix.
Fig. 4 is that recessed soil, recessed soil matrix molecular imprinting sorbing material and the sub-trace sorbing material of the non-molecule of recessed soil matrix are to CO
2adsorbance.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme of the present invention is described in further detail.Should be understood that these embodiments just in order to demonstrate the invention, but not limit the scope of the invention by any way.
Embodiment 1: prepare compound adsorbent according to following steps
(1) by attapulgite clay 105 DEG C of oven dry, pulverized 200 orders; Add attapulgite clay and the 100ml toluene of 3g oven dry in a reservoir, in whipping process, add 3ml silane coupler γ-(methacryloxypropyl) propyl trimethoxy silicane, react 50 minutes in 40 DEG C of ultrasonic waves; 5 hours are reacted again in the constant temperature oil bath of 40 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
(2) acrylamide of 2mmol and 1mmol acetic acid are placed in reactor, add the acetonitrile of 10mmol, sealing, ultrasonic disperse 10 minutes, whole system is fully dissolved mix, this system is left standstill 12 hours at ambient temperature, template molecule and function monomer is fully acted on, forms stable compound;
(3) in the template molecule-function monomer complex systems of above-mentioned step 2,10mmol crosslinking agent ethylene glycol dimethacrylate (EGDMA), 0.3mol initator azodiisobutyronitrile and 1g modified attapulgite clay is added, ultrasonic degas 10 minutes, after air is all replaced by logical nitrogen for 20 minutes, reactor is sealed, under 50 DEG C of constant temperatures, initiated polymerization 48 hours;
(4) polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with hydrochloric acid: methyl alcohol volume ratio is the mixed solvent cyclic washing 24 hours of 1:9, template molecule in removing product and other unreacted reactant, till can't detect the template in eluent with ultraviolet-uisible spectrophotometer, then with high purity water washing, 105 DEG C are drying to obtain described CO
2molecular imprinting absorbent.
Embodiment 2: prepare compound adsorbent according to following steps
(1) by attapulgite clay 105 DEG C of oven dry, pulverized 200 orders; Add attapulgite clay and the 120ml absolute ethyl alcohol of 3g oven dry in a reservoir, in whipping process, add 4ml silane coupler APTES, react 30 minutes in 45 DEG C of ultrasonic waves; 4 hours are reacted again in the constant temperature oil bath of 50 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
(2) acrylamide of 4mmol and 1mmol ethanedioic acid are placed in reactor, add the acetonitrile of 15mmol: volume of toluene is than the mixed solvent for 1:1, sealing, ultrasonic disperse 15 minutes, whole system is fully dissolved mix, this system is left standstill 24 hours at ambient temperature, template molecule and function monomer is fully acted on, forms stable compound;
(3) in the template molecule-function monomer complex systems of above-mentioned step 2,20mmol crosslinking agent ethylene glycol dimethacrylate (EGDMA), 0.4mol initator azodiisobutyronitrile and 1g modified attapulgite clay is added, ultrasonic degas 15 minutes, after air is all replaced by logical nitrogen for 15 minutes, reactor is sealed, under 60 DEG C of constant temperatures, initiated polymerization 24 hours;
(4) polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with hydrochloric acid: methyl alcohol volume ratio is the mixed solvent cyclic washing 30 hours of 1:9, template molecule in removing product and other unreacted reactant, till can't detect the template in eluent with ultraviolet-uisible spectrophotometer, then with high purity water washing, 105 DEG C are drying to obtain described CO
2molecular imprinting absorbent.
Embodiment 3: prepare compound adsorbent according to following steps
(1) by attapulgite clay 105 DEG C of oven dry, pulverized 200 orders; Add attapulgite clay and the 150ml toluene of 3g oven dry in a reservoir, in whipping process, add 5ml silane coupler APTES, react 30 minutes in 45 DEG C of ultrasonic waves; 3 hours are reacted again in the constant temperature oil bath of 60 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
(2) acrylamide of 8mmol and 1mmol ethanedioic acid are placed in reactor, add the acetonitrile solvent of 20mmol, sealing, ultrasonic disperse 20 minutes, whole system is fully dissolved mix, this system is left standstill 18 hours at ambient temperature, template molecule and function monomer is fully acted on, forms stable compound;
(3) in the template molecule-function monomer complex systems of above-mentioned step 2,30mmol crosslinking agent N is added, N '-methylene-bisacrylamide, 0.5mol initator azodiisobutyronitrile and 2g modified attapulgite clay, ultrasonic degas 20 minutes, after air is all replaced by logical nitrogen for 20 minutes, reactor is sealed, under 80 DEG C of constant temperatures, initiated polymerization 24 hours.
(4) polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with methanol solvate cyclic washing 36 hours, template molecule in removing product and other unreacted reactant, till can't detect the template in eluent with ultraviolet-uisible spectrophotometer, then with high purity water washing, 105 DEG C are drying to obtain described CO
2molecular imprinting absorbent.
Embodiment 4: prepare compound adsorbent according to following steps
(1) by attapulgite clay 105 DEG C of oven dry, pulverized 200 orders; Add attapulgite clay and the 150ml toluene of 3g oven dry in a reservoir, in whipping process, add 3ml silane coupler APTES, react 30 minutes in 45 DEG C of ultrasonic waves; 5 hours are reacted again in the constant temperature oil bath of 40 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
(2) acrylamide of 4mmol and 1mmol acetic acid are placed in reactor, add the toluene solvant of 20mmol, sealing, ultrasonic disperse 20 minutes, whole system is fully dissolved mix, this system is left standstill 24 hours at ambient temperature, template molecule and function monomer is fully acted on, forms stable compound;
(3) in the template molecule-function monomer complex systems of above-mentioned step 2,20mmol crosslinking agent EGDMA, 0.3mol initator azodiisobutyronitrile and 1g modified attapulgite clay is added, ultrasonic degas 20 minutes, after air is all replaced by logical nitrogen for 20 minutes, reactor is sealed, under 60 DEG C of constant temperatures, initiated polymerization 24 hours;
(4) polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with hydrochloric acid: methyl alcohol volume ratio is the mixed solvent cyclic washing 36 hours of 1:9, template molecule in removing product and other unreacted reactant, till can't detect the template in eluent with ultraviolet-uisible spectrophotometer, then with high purity water washing, 105 DEG C are drying to obtain described CO
2molecular imprinting absorbent.
Embodiment 5: prepare the non-molecular imprinting absorbent of recessed soil matrix according to following steps
(1) by attapulgite clay 105 DEG C of oven dry, pulverized 200 orders; Add attapulgite clay and the 150ml toluene of 3g oven dry in a reservoir, in whipping process, add 3ml silane coupler γ-(methacryloxypropyl) propyl trimethoxy silicane, react 30 minutes in 45 DEG C of ultrasonic waves; 3 hours are reacted again in the constant temperature oil bath of 60 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
(2) acrylamide of 4mmol is placed in reactor, adds the acetonitrile solvent of 20mmol, sealing, ultrasonic disperse 20 minutes, makes acrylamide fully dissolve;
(3) in the system of above-mentioned step 2,20mmol crosslinking agent EGDMA, 0.3mol initator azodiisobutyronitrile and 1g modified attapulgite clay is added, ultrasonic degas 20 minutes, after air is all replaced by logical nitrogen for 20 minutes, reactor is sealed, under 60 DEG C of constant temperatures, initiated polymerization 24 hours;
(4) polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with methanol solvate cyclic washing 24 hours, template molecule in removing product and other unreacted reactant, then with high purity water washing, 105 DEG C are drying to obtain the non-molecular imprinting absorbent of recessed soil matrix.
Claims (10)
1. recessed soil matrix molecular imprinting CO
2the preparation method of sorbing material, adopts silane coupler and attapulgite clay to react, carries out surface-functionalized, obtained modified attapulgite clay; Then initator, crosslinking agent, monomer and template are immersed in the duct of modified attapulgite clay, by initiated polymerization, in attapulgite clay duct, generate cross-linked polymer; Finally use eluting solvent eluted template, obtain the concavo-convex base molecular imprinting sorbing material with amidine functional group; It is characterized in that this molecular imprinting CO
2the preparation method of sorbing material comprises following concrete steps:
First step: by attapulgite clay 105 DEG C oven dry, pulverized 200 orders; Add attapulgite clay and the 100-150 weight parts organic solvent of 3 weight portions oven dry in a reservoir, in whipping process, add 3-5 weight portion silane coupler, in 40-45 DEG C of ultrasonic wave, react 30-50 minute; 3-5 hour is reacted again in the constant temperature oil bath of 40-60 DEG C of magnetic agitation; Product through the filtration of toluene, absolute ethyl alcohol and deionized water, washing, dry, pulverizing, obtains modified attapulgite clay successively;
Second step: the function monomer of 2-8mmol and 1mmol template molecule are placed in reactor, add 10-20mmol solvent, sealing, ultrasonic disperse 10-20 minute, makes whole system fully dissolve and mixes; This system is left standstill 12-24 hour at room temperature condition, template molecule and function monomer is fully acted on, forms stable compound;
Third step: add 10-30mmol crosslinking agent, 0.3-0.5mol initator and 1-2g modified attapulgite clay in the template molecule-function monomer complex systems of above-mentioned step 2, ultrasonic degas 10-20 minute, lead to after air all being replaced in inert gas 10-20 minute again, reactor is sealed, 50-80 DEG C of constant temperature initiated polymerization 24-48 hour;
4th step: step 3 polymeric reaction product is removed supernatant liquor, grinding and crossing 200 mesh sieves is placed in apparatus,Soxhlet's, with eluting solvent cyclic washing 24-36 hour, template molecule in removing product and other unreacted reactant, till can't detect the template in eluent with ultraviolet-uisible spectrophotometer, then with high purity water washing, 105 DEG C of dryings, obtain CO
2molecular imprinting absorbent.
2. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the coupling agent of employing is silane coupler: γ-(methacryloxypropyl) propyl trimethoxy silicane, APTES.
3. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the organic solvent adopted in first step is toluene or absolute ethyl alcohol.
4. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the template molecule of employing is acetic acid or ethanedioic acid.
5. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the function monomer of employing is acrylamide.
6. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the solvent that second step adopts is: acetonitrile, toluene, or the mixed solvent of acetonitrile and toluene; Wherein acetonitrile: the volume ratio of toluene is 1:1.
7. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the crosslinking agent of employing is ethylene glycol dimethacrylate (EGDMA), N, N '-methylene-bisacrylamide.
8. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the initator of employing is that azo-initiator is as azodiisobutyronitrile.
9. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: inert gas is nitrogen.
10. recessed soil matrix molecular imprinting CO according to claim 1
2the preparation method of sorbing material, is characterized in that: the eluting solvent adopted in the 4th step is: methyl alcohol, the mixed solvent of hydrochloric acid and methyl alcohol; Its hydrochloric acid: the volume ratio of methyl alcohol is 1:9.
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| CN109310981A (en) * | 2016-07-28 | 2019-02-05 | 南洋理工大学 | Composite material, its preparation and gas purification purposes |
| CN109894098A (en) * | 2017-12-07 | 2019-06-18 | 中国科学院宁波材料技术与工程研究所 | A kind of preparation method of polyamine base porous compound material |
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Application publication date: 20160309 |