CN116143959A - Preparation method of polyester material capable of efficiently adsorbing ammonia - Google Patents
Preparation method of polyester material capable of efficiently adsorbing ammonia Download PDFInfo
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- CN116143959A CN116143959A CN202310062081.7A CN202310062081A CN116143959A CN 116143959 A CN116143959 A CN 116143959A CN 202310062081 A CN202310062081 A CN 202310062081A CN 116143959 A CN116143959 A CN 116143959A
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- 229920000728 polyester Polymers 0.000 title claims abstract description 64
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 10
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims abstract description 41
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 36
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims abstract description 24
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010526 radical polymerization reaction Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 14
- 238000001291 vacuum drying Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 10
- 239000000706 filtrate Substances 0.000 claims description 8
- 229920000642 polymer Polymers 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 238000000967 suction filtration Methods 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 230000001681 protective effect Effects 0.000 claims description 2
- 239000002352 surface water Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 22
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 239000003463 adsorbent Substances 0.000 description 6
- 239000012621 metal-organic framework Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000005431 greenhouse gas Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002912 waste gas Substances 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 125000000686 lactone group Chemical group 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F122/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides or nitriles thereof
- C08F122/10—Esters
- C08F122/1006—Esters of polyhydric alcohols or polyhydric phenols, e.g. ethylene glycol dimethacrylate
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/18—Introducing halogen atoms or halogen-containing groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/34—Introducing sulfur atoms or sulfur-containing groups
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/20—Organic adsorbents
- B01D2253/202—Polymeric adsorbents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
- B01D2257/406—Ammonia
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of a polyester material capable of efficiently absorbing ammonia, which aims to prepare a material capable of efficiently absorbing ammonia, and comprises the following steps of firstly uniformly mixing trimethylolpropane trimethacrylate (TMPTMA), azodiisobutyronitrile (AIBN) and toluene in a conical flask, and preparing TMPTMA polyester through free radical polymerization; then, hydrochloric acid reacts with TMPTMA polyester to prepare HCl-TMPTMA polyester; finally, the polyester is prepared by the reaction of sulfuric acid and HCl-TMPTMA polyesterObtaining 0.05HCl-1H 2 SO 4 -TMPTMA polyester. The polyester material prepared by the invention has low cost and is prepared for NH 3 Is applied to NH with large adsorption capacity 3 Adsorbed high quality material.
Description
Technical Field
The invention relates to the field of waste gas treatment, in particular to a preparation method of a polyester material capable of efficiently adsorbing ammonia.
Background
Ammonia (NH) 3 ) Is a malodorous gas, also PM 2.5 Is one of the main precursors of (a) a polymer. The granular ammonium sulfate and ammonium nitrate converted in the atmosphere for PM 2.5 Contribution of (a) even exceeds NO x And is in an increasing situation year by year. According to the calculation of statistical annual-differentiation data of China, artificial source NH of 2022 China 3 The discharge amount is about 1360 ten thousand tons, however, NH 3 Is also an important resource and energy source, which fosters more than 40% of people worldwide as a nitrogenous fertilizer feedstock. But each year due to the large amount of NH produced 3 Causing global energy consumption and greenhouse gas emissions. If can waste human source NH 3 Adsorption recovery not only can protect air quality, but also can realize waste NH 3 Resource utilization, reduction of NH production 3 Resulting in greenhouse gas production and energy consumption. It can be seen that NH 3 The method is used as an energy resource and has good recovery value.
The adsorption method is a method for adsorbing by using porous materials (such as active carbon and molecular sieve), and mainly comprises the steps of intercepting, accumulating or concentrating one or more gases in mixed gas components on the surface of an adsorbent material according to the properties of the porous materials and the difference of adsorption selectivity of the materials on target gases. Therefore, the adsorption method can realize the separation of main gas components in malodorous gas, and the adsorbed gas can be desorbed from the adsorbent in a certain desorption mode later, thereby achieving the purposes of deodorizing, purifying and recycling the gas.
Activated carbon and Metal Organic Frameworks (MOFs) are used for NH adsorption 3 The adsorption mechanism of the conventional material of (2) can be divided into physical adsorption, hydrogen bonding and chemical adsorption. Due to NH 3 The molecular diameter of the catalyst is only 3A DEG, and the active carbon with high specific surface area and large pore volume can not effectively capture NH through physical adsorption 3 . To strengthen NH 3 Adsorption, usually by material design or modification method, of-COOH, -OH, -SO 3 Oxygen-containing functional groups such as H or lactone groups, adsorbing NH by hydrogen bonding or acid-base action 3 . However, extensive research has shown that the optimized activated carbon pair NH 3 The adsorption amount of (2) is still not satisfactory. In addition, waste gas or waste liquid is often generated in the modification process (such as high temperature and solvent treatment) of the activated carbon, so that secondary pollution is caused. MOFs vs NH 3 Has better removal effect. However, MOFs are costly and limit their use. MOFs are reported to be tens of thousands times more expensive than activated carbon. Therefore, low cost, high adsorption capacity NH was developed 3 Adsorbent for waste NH 3 The efficient adsorption and separation of (2) becomes a key to break through the application limitations. In view of the above problems, a solution is proposed below.
Disclosure of Invention
The invention aims to provide a preparation method of a polyester material capable of efficiently adsorbing ammonia gas, which has the advantages of low cost and large adsorption capacity of the obtained polyester material.
The technical aim of the invention is realized by the following technical scheme:
a method for preparing a polyester material capable of efficiently adsorbing ammonia gas comprises the following steps,
(1) Preparation of TMPTMA polyesters
S1: uniformly mixing trimethylolpropane trimethacrylate (TMPTMA), azobisisobutyronitrile (AIBN) and toluene in a conical flask, wherein the ratio of the trimethylolpropane trimethacrylate (mL), toluene (mL) and AIBN (mg) is 1:10:30, and stirring the mixed solution until AIBN solid is completely dissolved in the trimethylolpropane trimethacrylate and toluene;
s2: introducing protective gas into the conical flask to completely exhaust air in the conical flask, and sealing the conical flask by using aluminum foil to isolate the air;
s3: placing the sealed conical flask in an electric constant-temperature water bath at 60 ℃ for 24 hours, and performing free radical polymerization reaction, wherein in the reaction, the precipitate in toluene is an adsorbent precursor;
s4: after the free radical polymerization reaction is completed, carrying out suction filtration on the polymer, removing liquid on the surface of a filter material, and then placing the filter material in a vacuum drying oven for drying to obtain TMPTMA polyester;
(2) Preparation of 0.05HCl-TMPTMA polyester
S5: placing a proper amount of TMPTMA polyester into a conical flask, adding a proper amount of hydrochloric acid, sealing the conical flask, and placing the conical flask into a magnetic stirrer for stirring;
s6: filtering the polyester in the conical flask to remove water on the surface, and then placing the filtrate in a vacuum drying oven to dry to obtain 0.05HCl-TMPTMA polyester;
(3) Preparation of 0.05HCl-1H 2 SO 4 The polyester of TMPTMA,
s7: putting a proper amount of polymer 0.05HCl-TMPTMA polyester into a conical flask, adding a proper amount of sulfuric acid, and then putting the conical flask into a magnetic stirrer for stirring;
s8: filtering polyester in conical flask to remove surface water, and drying the filtrate in vacuum drying oven to obtain 0.05HCl-1H 2 SO 4 -TMPTMA polyester.
Preferably, the operation of evacuating the air in the conical flask in step S2 is as follows: a shielding gas, which is high purity nitrogen, is introduced into the conical flask for 10 min.
Preferably, when the vacuum drying oven dries the filtrate in the steps S4, S6 and S8, the temperature in the vacuum drying oven is 85 ℃ and the drying time is 24 hours.
Preferably, the rotation speed of the magnetic stirrer in the step S5 and the step S7 is 750r/min, and the stirring time period is 24h.
Preferably, in the step S5, the amount of TMPTMA polyester is 2g, the amount of hydrochloric acid is 250ml, and the concentration of hydrochloric acid is 0.05mol/L.
Preferably, the amount of the 0.05HCl-TMPTMA polyester in the step S7 is 2g, the amount of the sulfuric acid is 250mL, and the concentration of the sulfuric acid is 1mol/L.
The beneficial effects of the invention are as follows: 0.05HCl-1H prepared by the scheme 2 SO 4 The TMPTMA polyester material can efficiently absorb ammonia and can be recycled. And the cost in the manufacturing process is low, the method can be greatly popularized and applied, and the method is a high-quality material for adsorbing ammonia.
Drawings
FIG. 1 is a schematic representation of NH adsorption by TMPTMA polyester in example 3 3 Is a device diagram of (a).
Reference numerals: 1. a mass flow controller; 2. a mixing tank; 3. pumping NH 3 And a detector.
Detailed Description
The following description is only of the preferred embodiments of the present invention, and the scope of the present invention should not be limited to the examples, but should be construed as falling within the scope of the present invention.
Example 1: preparation of TMPTMA polyesters
1. TMPTMA, AIBN and toluene were mixed uniformly in a conical flask in a ratio of TMPTMA (mL): toluene (mL): AIBN (mg) =1:10:30. Stirring the solution until the AIBN solid is completely dissolved in TMPTMA and toluene;
2. introducing high-purity nitrogen into the conical flask for 10min, and sealing the conical flask by using aluminum foil to isolate air after the air in the conical flask is completely discharged;
3. placing the conical flask in an electric constant-temperature water bath at 60 ℃ for 24 hours to complete free radical polymerization reaction, and separating out an adsorbent precursor from toluene in the process;
4. after the reaction is finished, the polymer is subjected to suction filtration to remove liquid on the surface of the polymer, the filtrate is placed in a vacuum drying oven at 85 ℃ for 24 hours, the moisture is thoroughly removed to obtain TMPTMA polyester, and the TMPTMA polyester is placed in a dryer for standby.
Example 2: preparation of 0.05HCl-TMPTMA, 0.25HCl-TMPTMA, 1.25HCl-TMPTMA, 6.25HCl-TMPTMA polyester
1.2 g of prepared TMPTMA is put into a conical flask, 0.05mol/L, 0.25mol/L, 1.25mol/L and 6.25mol/L of hydrochloric acid are respectively added into 250mL, and the mixture is placed into a magnetic stirrer in a sealing way and stirred for 24h at a rotating speed of 750 r/min;
2. and (3) carrying out suction filtration on the TMPTMA polyester in the conical flask to remove water on the surface of the TMPTMA polyester, and then placing the filtrate in a vacuum drying oven at 85 ℃ for 24 hours to thoroughly remove water to obtain 0.05HCl-TMPTMA, 0.25HCl-TMPTMA, 1.25HCl-TMPTMA and 6.25HCl-TMPTMA polyester.
Example 3: NH (NH) 3 Dynamic adsorption experiments
Adsorption of NH by TMPTMA polyester 3 As shown in the figure. 1 is a control panel, 2 is a gas mixing tank, an adsorption column and 3 is NH 3 And a detector. Wherein N is 2 The flow rate of (C) is 180mL/min, NH 3 The flow rate of (C) is 20mL/min, N 2 The concentration of (C) is 99.999%, NH 3 The concentration of (2) was 5000ppm, and the amount of the adsorbent used in the adsorption test was 0.2g.
TABLE 1 TMPTMA polyester vs. NH after different hydrochloric acid concentration control 3 Dynamic adsorption capacity
Example 4:1H 2 SO 4 Preparation of TMPTMA polyesters
1.2 g of the prepared TMPTMA polyester is put into a conical flask, 250mL of 1mol/L sulfuric acid is added, and stirring is carried out for 24 hours at the rotating speed of 750r/min by a magnetic stirrer;
2. filtering TMPTMA polyester in conical flask to remove water on its surface, and vacuum drying at 85deg.C for 24 hr to thoroughly remove water to obtain 1H 2 SO 4 -TMPTMA polyester.
Example 5:0.05HCl-1H 2 SO 4 Preparation of TMPTMA polyesters
1.2 g of the prepared polymer 0.05HCL-TMPTMA polyester is put into a conical flask, 250mL of 1mol/L sulfuric acid is added, and the mixture is stirred for 24 hours at a rotating speed of 750r/min by a magnetic stirrer;
2. filtering the polyester in the conical flask to remove water on the surface of the polyester, placing the filtrate in a vacuum drying oven at 85deg.C for 24 hr, and thoroughly removing water to obtain 0.05HCl-1H 2 SO 4 -TMPTMA polyester.
TABLE 2 TMPTMA polyester vs NH after hydrochloric acid or sulfuric acid control 3 Dynamic adsorption capacity
The technical problems, technical solutions and advantageous effects solved by the present invention have been further described in detail in the above-described embodiments, and it should be understood that the above-described embodiments are only illustrative of the present invention and are not intended to limit the present invention, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the scope of protection of the present invention.
Claims (6)
1. A preparation method of a polyester material capable of efficiently adsorbing ammonia is characterized by comprising the following steps of,
(1) Preparation of TMPTMA polyesters
S1: uniformly mixing trimethylolpropane trimethacrylate (TMPTMA), azobisisobutyronitrile (AIBN) and toluene in a conical flask, wherein the ratio of the trimethylolpropane trimethacrylate (mL), toluene (mL) and AIBN (mg) is 1:10:30, and stirring the mixed solution until AIBN solid is completely dissolved in the trimethylolpropane trimethacrylate and toluene;
s2: introducing protective gas into the conical flask to completely exhaust air in the conical flask, and sealing the conical flask by using aluminum foil to isolate the air;
s3: placing the sealed conical flask in an electric constant-temperature water bath at 60 ℃ for 24 hours, and carrying out free radical polymerization reaction;
s4: after the free radical polymerization reaction is completed, carrying out suction filtration on the polymer, removing liquid on the surface of a filter material, and then placing the filter material in a vacuum drying oven for drying to obtain TMPTMA polyester;
(2) Preparation of 0.05HCl-TMPTMA polyester
S5: placing a proper amount of TMPTMA polyester into a conical flask, adding a proper amount of hydrochloric acid, sealing the conical flask, and placing the conical flask into a magnetic stirrer for stirring;
s6: filtering the polyester in the conical flask to remove water on the surface, and then placing the filtrate in a vacuum drying oven to dry to obtain 0.05HCl-TMPTMA polyester;
(3) Preparation of 0.05HCl-1H 2 SO 4 The polyester of TMPTMA,
s7: putting a proper amount of 0.05HCl-TMPTMA polyester into a conical flask, adding a proper amount of sulfuric acid, and then putting the conical flask into a magnetic stirrer for stirring;
s8: filtering polyester in conical flask to remove surface water, and drying the filtrate in vacuum drying oven to obtain 0.05HCl-1H 2 SO 4 -TMPTMA polyester.
2. The method for preparing a polyester material capable of efficiently adsorbing ammonia gas according to claim 1, wherein the operation of evacuating the air in the conical flask in step S2 is as follows: a shielding gas, which is high purity nitrogen, is introduced into the conical flask for 10 min.
3. The method for preparing a polyester material capable of efficiently adsorbing ammonia gas according to claim 1, wherein when the filter is dried by the vacuum drying oven in the steps S4, S6 and S8, the temperature in the vacuum drying oven is 85 ℃ and the drying time is 24 hours.
4. The method for preparing the polyester material capable of efficiently adsorbing ammonia according to claim 1, wherein the rotation speed of the magnetic stirrer in the step S5 and the step S7 is 750r/min, and the stirring time is 24h.
5. The method for preparing a polyester material capable of efficiently adsorbing ammonia gas according to claim 1, wherein in the step S5, the amount of TMPTMA polyester is 2g, the amount of hydrochloric acid is 250mL, and the concentration of hydrochloric acid is 0.05mol/L.
6. The method for preparing a polyester material capable of efficiently adsorbing ammonia gas according to claim 1, wherein the amount of 0.05HCl-TMPTMA polyester used in the step S7 is 2g, the amount of sulfuric acid is 250mL, and the sulfuric acid concentration is 1mol/L.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01258740A (en) * | 1988-04-07 | 1989-10-16 | Japan Atom Energy Res Inst | Production of adsorbent for gas |
| CN1349420A (en) * | 1999-04-29 | 2002-05-15 | 巴斯福股份公司 | Superabsorbent polymer containing odor controlling compounds |
| CN110467707A (en) * | 2018-05-10 | 2019-11-19 | 北京工业大学 | A kind of method of modifying effectively improving MOFs water stability and ammonia gas absorption performance |
-
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- 2023-01-18 CN CN202310062081.7A patent/CN116143959A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01258740A (en) * | 1988-04-07 | 1989-10-16 | Japan Atom Energy Res Inst | Production of adsorbent for gas |
| CN1349420A (en) * | 1999-04-29 | 2002-05-15 | 巴斯福股份公司 | Superabsorbent polymer containing odor controlling compounds |
| CN110467707A (en) * | 2018-05-10 | 2019-11-19 | 北京工业大学 | A kind of method of modifying effectively improving MOFs water stability and ammonia gas absorption performance |
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