CN111389215A - Preparation method and application of hyperbranched polyamide modified activated carbon - Google Patents
Preparation method and application of hyperbranched polyamide modified activated carbon Download PDFInfo
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- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/72—Organic compounds not provided for in groups B01D53/48 - B01D53/70, e.g. hydrocarbons
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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
Abstract
The invention provides a preparation method of hyperbranched polyamide modified activated carbon, which comprises the steps of boiling activated carbon with deionized water, rinsing, and then drying in vacuum to obtain pretreated activated carbon AC; adding the pretreated activated carbon AC into an acid solution, reacting for 6-8H at 60-70 ℃, filtering, washing, and drying in vacuum to obtain acidified activated carbon AC-H; adding acidified activated carbon AC-H into a hyperbranched polyamide aqueous solution, uniformly stirring and dispersing, adding a water shrinking agent N, N-dicyclohexylcarbodiimide, reacting for 4-6H at 70-80 ℃, washing, and drying in vacuum to obtain the hyperbranched polyamide modified activated carbon. The hyperbranched polyamide modified activated carbon is used for purifying formaldehyde in air, combines two functions of physical adsorption and chemical decomposition, has a very good enriching and decomposing effect on formaldehyde, can efficiently remove formaldehyde in air, avoids the risk of secondary pollution, and can effectively solve the pollution problem of indoor formaldehyde.
Description
Technical Field
The invention relates to a preparation method of hyperbranched polyamide modified activated carbon, and also relates to application of the hyperbranched polyamide modified activated carbon in purifying formaldehyde in air, belonging to the technical field of carbon materials and air purification.
Background
With the rapid development of social economy, the living standard of people is continuously improved, and the people are in right positionThe concept of health and environmental protection is becoming more and more intense, wherein the problem of air quality of residential environment becomes a hot topic of concern. Formaldehyde is one of the main pollutants affecting indoor air quality, and is generally present in various building materials such as artificial boards, adhesives, wooden furniture, wallpaper and the like. Formaldehyde has strong stimulation to human skin and organs, and can cause various diseases such as dermatitis, asthma and the like in severe cases, and even has the risk of cancer. China 'indoor air quality Standard' stipulates: the limit value of formaldehyde in indoor air of civil building engineering such as houses, hospitals, classrooms of schools, old buildings, kindergartens and the like is 0.08mg/m3. The common methods for treating the formaldehyde exceeding standard at present comprise: biological decomposition method (chlorophytum comosum and scindapsus aureus, etc.), physical adsorption method (active carbon, attapulgite, etc.), photocatalytic decomposition method (nano titanium dioxide), and aldehyde removal technology for various modified materials. The biological decomposition method is subject to multiple factors such as weather, temperature and the like, and cannot ensure high-efficiency formaldehyde removing efficiency. The physical adsorption method is the most commonly used method, but the defect of adsorption saturation limits better application of the method, and the nano titanium dioxide photocatalyst catalytic decomposition method can efficiently decompose formaldehyde only under ultraviolet radiation and is not suitable for treating high-concentration formaldehyde. Researchers prepare various modified materials according to a mode of combining different methods, and the modified materials have obvious advantages compared with a single formaldehyde removal technology, wherein the modified adsorption materials represented by amine modified activated carbon are synergistic by a physical adsorption method and a chemical decomposition method, so that the modified adsorption materials have the advantages of large adsorption capacity, high adsorption speed and reduction of the risk of secondary pollution, and become a hotspot of research of technicians.
The amine modified activated carbon adsorption material firstly adsorbs and enriches formaldehyde on the surface of activated carbon, and then performs chemical reaction with grafted amine, thereby efficiently removing formaldehyde in the environment. The number of amino groups chemically grafted with activated carbon also directly determines the formaldehyde-removing efficiency of the activated carbon, and researches (Li Kun power, Yangmen, Wang Yanjin, et al. preparation of novel aminated mesoporous carbon and adsorption of the novel aminated mesoporous carbon to Pb (II) [ J ]. Chinese environmental science, 2014, 34(8): 1985-1992.) report the technology of grafting activated carbon with small molecules such as ethylenediamine and the like, but the material has low formaldehyde removal efficiency and still has the risk of secondary pollution, and the development of a high-molecular polyamine polymer grafted activated carbon adsorption material can effectively solve the problems. The formaldehyde removal technology of the polyhydrazide grafted activated carbon material is reported by research (Zhang Yi' an, Dixifeng, preparation of the polyhydrazide grafted and modified activated carbon material and influence factors thereof [ J ]. environmental science research, 31 (8)), but the industrial application of the material is limited by factors such as complex synthetic process of the polyhydrazide, relatively high cost and the like. The amino-terminated hyperbranched polyamide is a highly branched polymer, the molecular structure of the hyperbranched polyamide contains a large number of terminal amino functional groups, and the hyperbranched polyamide has unique advantages in the aspects of reactivity, solubility and the like. Hyperbranched polyamides with different molecular weights can be prepared by different synthesis processes, so that the hyperbranched polyamides can be widely applied to novel chemical materials, and the modification technology of activated carbon by using the hyperbranched polyamides with terminal amino groups is not reported.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a preparation method of hyperbranched polyamide modified activated carbon.
The invention also aims to provide the hyperbranched polyamide modified activated carbon prepared by the preparation method for purifying formaldehyde in indoor air.
The invention relates to a preparation method of hyperbranched polyamide modified activated carbon, which comprises the following steps:
(1) boiling and rinsing the activated carbon by using deionized water, and then drying the activated carbon in vacuum to obtain pretreated activated carbon AC;
(2) adding the pretreated activated carbon AC obtained in the step (1) into an acid solution, reacting for 6-8H at 60-70 ℃, filtering, washing, and drying in vacuum to obtain acidified activated carbon AC-H;
(3) adding acidified activated carbon AC-H into a hyperbranched polyamide aqueous solution, uniformly stirring and dispersing, adding a water shrinking agent N, N-dicyclohexylcarbodiimide, reacting for 4-6H at 70-80 ℃, washing, and drying in vacuum to obtain the hyperbranched polyamide modified activated carbon.
In the step (1), the activated carbon is one of coconut shell activated carbon, shell activated carbon or coal activated carbon; the particle size of the activated carbon is 0.44-0.50 mm.
In the step (1), the vacuum drying temperature is 100-110 ℃, and the time is 20-24 h.
In the step (2), the acid solution is one of a nitric acid solution or a sulfuric acid solution or a mixed solution of the nitric acid solution and the sulfuric acid solution; the mass concentration of the acid solution is 15-30%.
In the step (2), the vacuum drying temperature is 100-110 ℃, and the time is 10-12 h.
In the step (3), the molecular weight of the hyperbranched polyamide is 1800-2200 g/mol, and the preparation method comprises the following steps: taking triethylenetetramine and methyl acrylate as raw materials, taking methanol as a solvent, reacting at room temperature for 20-24 h, then gradually heating to 30 ℃, 60 ℃, 90 ℃, 120 ℃, keeping the negative pressure at 0.05MPa, recovering the methanol in a water separator in time, and carrying out heat preservation reaction at each temperature point for 2h to obtain a yellow viscous polymerization product, namely hyperbranched polyamide; wherein the molar ratio of the methyl acrylate to the triethylene tetramine is as follows: 0.7:1 to 1.2: 1.
In the step (3), the mass ratio of the hyperbranched polyamide aqueous solution to the acidified activated carbon AC-H is 50: 1-100: 1, and the concentration of the hyperbranched polyamide aqueous solution is 15-25 g/L.
In the step (3), the adding amount of the N, N-dicyclohexylcarbodiimide is 1.0-1.5% of the mass of the acidified activated carbon AC-H.
In the step (3), the vacuum drying temperature is 90-100 ℃, and the time is 5-6 h.
The hyperbranched polyamide modified activated carbon prepared by the invention is subjected to formaldehyde purification test, and has good removal rate on formaldehyde under the conditions that the ambient temperature is 5-50 ℃ and the relative humidity is 35-60%, which indicates that the hyperbranched polyamide modified activated carbon is applicable to normal environment. According to the detection data of a gas-phase formaldehyde test method (a reaction chamber detection method), the average removal rate of formaldehyde by the hyperbranched polyamide modified activated carbon under the conditions of the environmental temperature and the relative humidity is 94.3 percent, the average removal rate of formaldehyde by the ethylenediamine modified activated carbon is 79.8 percent, and the average removal rate of formaldehyde by the unmodified activated carbon is 52 percent. The hyperbranched polyamide modified activated carbon has good effect on removing formaldehyde in the air.
In conclusion, the hyperbranched polyamide is used for modifying the activated carbon, so that the operation is simple, the cost is lower, and the application range is wide. The prepared hyperbranched polyamide modified activated carbon combines two functions of physical adsorption and chemical decomposition, formaldehyde is firstly adsorbed and enriched on the surface of the activated carbon and then reacts with hyperbranched polyamide through Schiff base reaction, and the reaction has the advantages of high response speed, easiness in control and the like, and can efficiently decompose formaldehyde in the environment. Compared with a single physical adsorption or chemical decomposition technology, the hyperbranched polyamide modified activated carbon technology has the advantages of large adsorption capacity, high formaldehyde removal efficiency, difficult formaldehyde desorption and the like, avoids the risk of secondary pollution, can effectively solve the problem of indoor formaldehyde pollution, and has very good social benefit.
Detailed Description
The preparation and use of the hyperbranched polyamide-modified activated carbon of the invention are further illustrated by the following specific examples.
Example 1
(1) Weighing 10g of coconut shell activated carbon with the particle size of 0.44-0.50 mm, adding the coconut shell activated carbon into a flask filled with 200m L deionized water, boiling for 0.5h, filtering, rinsing with the deionized water for 2-3 times, performing suction filtration, and performing vacuum drying at 110 ℃ for 24h to obtain pretreated activated carbon AC;
(2) adding the AC obtained in the step (1) into a three-necked bottle filled with an acid solution (prepared by sulfuric acid and nitric acid in a ratio of 1: 1) with the concentration of 200m L and the concentration of 20%, reacting for 6H at the temperature of 60 ℃, filtering, washing with deionized water to be neutral, and drying in vacuum for 12H at the temperature of 110 ℃ to obtain acidified active carbon AC-H;
(3) weighing 42.11g (0.288 mol) of triethylenetetramine, dissolving with 46.1g (1.44 mol) of methanol, transferring to a three-necked bottle, stirring uniformly, dropwise adding 25.65g (0.298 mol) of methyl acrylate, reacting at room temperature for 24h, gradually heating to 30 ℃, 60 ℃, 90 ℃, 120 ℃, keeping the negative pressure at 0.05MPa, recovering the methanol in a water separator in time, and reacting at each temperature point for 2h to obtain a yellow viscous polymerization product, namely hyperbranched polyamide;
(4) adding 500g of 20 g/L g hyperbranched polyamide aqueous solution into a 1000m L three-necked bottle, adding 8.0g of acidified active carbon AC-H, starting mechanical stirring, adding 0.12g of N, N-dicyclohexylcarbodiimide after uniform dispersion, reacting for 4-6H at 80 ℃, washing the product for 2-3 times, and vacuum drying for 6H at 90 ℃ to obtain the hyperbranched polyamide modified active carbon.
The formaldehyde purification performance of the product is inspected by a gas-phase formaldehyde test method (reaction chamber detection method), the average formaldehyde removal rate is 94.3% under the conditions that the ambient temperature is 5-50 ℃ and the relative humidity is 35-60%, and the influence of the ambient conditions on the formaldehyde removal rate is small.
Example 2
(1) Weighing 10g of coconut shell activated carbon with the particle size of 0.44-0.50 mm, adding the coconut shell activated carbon into a flask filled with 200m L deionized water, boiling for 0.5h, filtering, rinsing with the deionized water for 2-3 times, performing suction filtration, and performing vacuum drying at 110 ℃ for 24h to obtain pretreated activated carbon AC;
(2) adding the AC obtained in the step (1) into a three-necked bottle filled with a sulfuric acid solution with the concentration of 200m L being 30%, reacting for 6H at the temperature of 60 ℃, filtering, washing with deionized water to be neutral, and vacuum drying for 12H at the temperature of 110 ℃ to obtain acidified active carbon AC-H;
(3) weighing 42.11g (0.288 mol) of triethylenetetramine, dissolving with 46.1g (1.44 mol) of methanol, transferring to a three-necked bottle, stirring uniformly, dropwise adding 28.58g (0.332 mol) of methyl acrylate, reacting at room temperature for 24h, gradually heating to 30 ℃, 60 ℃, 90 ℃, 120 ℃, keeping the negative pressure at 0.05MPa, recovering the methanol in a water separator in time, and reacting at each temperature point for 2h to obtain a yellow viscous polymer product, namely hyperbranched polyamide;
(4) adding 700g of hyperbranched polyamide aqueous solution with the concentration of 20 g/L into a 1000m L three-necked bottle, adding 9.0g of acidified activated carbon AC-H, starting mechanical stirring, adding 0.10g of N, N-dicyclohexylcarbodiimide after uniform dispersion, reacting for 4-6H at 80 ℃, washing the product for 2-3 times with water, and drying for 6H at 90 ℃ in vacuum to obtain the hyperbranched polyamide modified activated carbon.
The formaldehyde purification performance of the product is inspected by a gas-phase formaldehyde test method (reaction chamber detection method), the average formaldehyde removal rate is 91.2% under the conditions that the ambient temperature is 5-50 ℃ and the relative humidity is 35-60%, and the influence of the ambient conditions on the formaldehyde removal rate is small.
Example 3
(1) Weighing 20g of coconut shell activated carbon with the particle size of 0.44-0.50 mm, adding the coconut shell activated carbon into a flask filled with 400m L deionized water, boiling for 0.5h, filtering, rinsing with the deionized water for 2-3 times, performing suction filtration, and performing vacuum drying at 110 ℃ for 24h to obtain pretreated activated carbon AC;
(2) adding the AC obtained in the step (1) into a three-necked bottle filled with a nitric acid solution with the concentration of 400m L being 15%, reacting for 6H at the temperature of 60 ℃, filtering, washing with deionized water to be neutral, and vacuum drying for 12H at the temperature of 110 ℃ to obtain acidified active carbon AC-H;
(3) weighing 42.11g (0.288 mol) of triethylenetetramine, dissolving with 46.1g (1.44 mol) of methanol, transferring to a three-necked bottle, stirring uniformly, dropwise adding 24.28g (0.282 mol) of methyl acrylate, reacting at room temperature for 24h, gradually heating to 30 ℃, 60 ℃, 90 ℃, 120 ℃, keeping the negative pressure at 0.05MPa, recovering the methanol in a water separator in time, and reacting at each temperature point for 2h to obtain a yellow viscous polymer product, namely hyperbranched polyamide;
(4) adding 1000g of hyperbranched polyamide aqueous solution with the concentration of 20 g/L into a 2000m L three-necked bottle, adding 15.0g of acidified active carbon AC-H, starting mechanical stirring, adding 0.15g of N, N-dicyclohexylcarbodiimide after uniform dispersion, reacting for 4-6H at 80 ℃, washing the product for 2-3 times with water, and drying for 6H at 90 ℃ in vacuum to obtain the hyperbranched polyamide modified active carbon.
The formaldehyde purification performance of the product is inspected by a gas-phase formaldehyde test method (reaction chamber detection method), the average formaldehyde removal rate is 92.7% at the ambient temperature of 5-50 ℃ and the relative humidity of 35-60%, and the influence of the environmental conditions on the formaldehyde removal rate is small.
Claims (10)
1. A preparation method of hyperbranched polyamide modified activated carbon is characterized by comprising the following steps: the method comprises the following steps:
(1) boiling and rinsing the activated carbon by using deionized water, and then drying the activated carbon in vacuum to obtain pretreated activated carbon AC;
(2) adding the pretreated activated carbon AC obtained in the step (1) into an acid solution, reacting for 6-8H at 60-70 ℃, filtering, washing, and drying in vacuum to obtain acidified activated carbon AC-H;
(3) adding acidified activated carbon AC-H into a hyperbranched polyamide aqueous solution, uniformly stirring and dispersing, adding a water shrinking agent N, N-dicyclohexylcarbodiimide, reacting for 4-6H at 70-80 ℃, washing, and drying in vacuum to obtain the hyperbranched polyamide modified activated carbon.
2. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (1), the activated carbon is one of coconut shell activated carbon, shell activated carbon or coal activated carbon; the particle size of the activated carbon is 0.44-0.50 mm.
3. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (1), the vacuum drying temperature is 100-110 ℃, and the time is 20-24 h.
4. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (2), the acid solution is one of a nitric acid solution or a sulfuric acid solution or a mixed solution of the nitric acid solution and the sulfuric acid solution; the mass concentration of the acid solution is 15-30%.
5. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (2), the vacuum drying temperature is 100-110 ℃, and the time is 10-12 h.
6. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (3), the molecular weight of the hyperbranched polyamide is 1800-2200 g/mol, and the preparation method comprises the following steps: taking triethylenetetramine and methyl acrylate as raw materials, taking methanol as a solvent, reacting at room temperature for 20-24 h, then gradually heating to 30 ℃, 60 ℃, 90 ℃, 120 ℃, keeping the negative pressure at 0.05MPa, recovering the methanol in a water separator in time, and carrying out heat preservation reaction at each temperature point for 2h to obtain a yellow viscous polymerization product, namely hyperbranched polyamide; wherein the molar ratio of the methyl acrylate to the triethylene tetramine is as follows: 0.7:1 to 1.2: 1.
7. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein in the step (3), the mass ratio of the hyperbranched polyamide aqueous solution to the acidified activated carbon AC-H is 50: 1-100: 1, and the concentration of the hyperbranched polyamide aqueous solution is 15-25 g/L.
8. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (3), the adding amount of the N, N-dicyclohexylcarbodiimide is 1.0-1.5% of the mass of the acidified activated carbon AC-H.
9. The preparation method of the hyperbranched polyamide modified activated carbon according to claim 1, wherein the preparation method comprises the following steps: in the step (3), the vacuum drying temperature is 90-100 ℃, and the time is 5-6 h.
10. The hyperbranched polyamide modified activated carbon prepared by the method of claim 1 is used for purifying formaldehyde in air.
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