CN109999760B - Active carbon loaded macroporous adsorption resin and preparation method thereof - Google Patents
Active carbon loaded macroporous adsorption resin and preparation method thereof Download PDFInfo
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- CN109999760B CN109999760B CN201811300471.9A CN201811300471A CN109999760B CN 109999760 B CN109999760 B CN 109999760B CN 201811300471 A CN201811300471 A CN 201811300471A CN 109999760 B CN109999760 B CN 109999760B
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- 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
- B01J20/02—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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- 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
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- B01J20/265—Synthetic macromolecular compounds modified or post-treated polymers
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
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- C08F2/18—Suspension polymerisation
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers 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 an aromatic carbocyclic ring
- C08F212/02—Monomers containing only one unsaturated aliphatic radical
- C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F212/06—Hydrocarbons
- C08F212/08—Styrene
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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
- C08F212/00—Copolymers 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 an aromatic carbocyclic ring
- C08F212/34—Monomers containing two or more unsaturated aliphatic radicals
- C08F212/36—Divinylbenzene
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Abstract
The invention discloses an active carbon loaded macroporous adsorption resin and a preparation method thereof, wherein active carbon is loaded on a resin framework by utilizing an organic carbon source by virtue of a stable framework of the resin, the adsorption selectivity of the prepared macroporous adsorption resin is improved, the organic carbon source is adopted as an active carbon raw material in the preparation method, the problem of severe preparation environment caused by using powdered active carbon is avoided, firstly, an oil phase obtained by mixing a monomer, a cross-linking agent and a pore-forming agent is added into a water phase, a suspension polymerization method is adopted for synthesis and extraction to obtain resin spheres, then, the organic carbon source is adsorbed to the resin spheres through a column, and after a high-pressure hydrothermal reaction, the active carbon is loaded on the resin framework, so that the macroporous adsorption resin is prepared.
Description
Technical Field
The invention belongs to the technical field of high polymer separation materials, relates to macroporous adsorption resin and a preparation method thereof, and particularly relates to active carbon loaded macroporous adsorption resin and a preparation method thereof.
Background
Macroporous adsorption resin is a high molecular separation material developed in the sixties and seventies of the last century, is used as an artificial synthetic material, and has the characteristics of large adsorption capacity, easy resolution, high strength and long service life compared with the traditional material such as activated carbon. For decades, research into adsorption resins has been done with great success. The application of the adsorption resin is gradually expanded to more fields. In the research on the adsorption resin, how to improve the selectivity of adsorption is always a constantly sought-after goal. It has been preliminarily ascertained that the adsorption mechanism is mainly through hydrophobic adsorption, delocalized pi-electron adsorption and hydrogen bond adsorption, and the more unitary the adsorption mechanism is, the higher the adsorption selectivity is. Since hydrogen bonds are widely found in nature, hydrogen bond adsorption has been studied in a series and has actually been used.
The activated carbon is used as a natural adsorption material, more than 80-90% of the activated carbon is composed of carbon elements, has strong hydrophobicity, has the advantages of good adsorption performance, strong decoloring and deodorizing capabilities, economy, durability and the like, is widely applied to industries of food, beverage, medicine, tap water, sugar, grease and the like, and is also commonly applied to the fields of wine brewing, sewage treatment, power plants, electroplating and the like. Therefore, the activated carbon is loaded into the macroporous adsorption resin, so that the adsorption selectivity of the macroporous adsorption resin is improved to a great extent, and the performance of the macroporous adsorption resin is further improved.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an activated carbon-loaded macroporous adsorption resin and a preparation method thereof.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of macroporous adsorption resin loaded with activated carbon comprises the following steps:
s1, mixing a monomer, a cross-linking agent and a pore-foaming agent to obtain an oil phase, adding a water phase into a container, heating, adding the oil phase into the water phase, synthesizing by a suspension polymerization method, and extracting by a solvent to obtain a resin ball;
s2, allowing the resin balls to pass through a column to adsorb an organic carbon source, wherein the organic carbon source is at least one of a sucrose solution, a glucose solution, a fructose solution, a galactose solution, a lactose solution and a maltose solution;
and S3, adding the resin balls adsorbed with the organic carbon source into distilled water to perform high-pressure hydrothermal reaction, and obtaining the active carbon loaded macroporous adsorption resin.
The monomer includes at least one of styrene, methyl acrylate and acrylonitrile, the crosslinking agent includes divinylbenzene, the porogen includes at least one of white oil, liquid paraffin, solid paraffin, polystyrene and polymethyl acrylate, and the aqueous phase includes distilled water.
In the step S1, the oil phase comprises, by mass, 1-10 parts of a monomer, 1-10 parts of a cross-linking agent and 2-5 parts of a pore-forming agent, and the water phase is 20-30 parts.
And S1, adding the water phase into a container, heating to 45-55 ℃, then uniformly mixing the oil phase, adding the oil phase into the water phase, heating to 65-75 ℃ for reaction for 3-8h, continuing heating to 85-95 ℃ for reaction for 3-10h, cooling to obtain intermediate resin, finally extracting the intermediate resin with a solvent, and after extraction, sequentially washing with distilled water at 90 ℃ or higher, boiling with water and drying to obtain the resin spheres.
When the solvent is used for extracting the intermediate resin in the step S1, the volume ratio of the solvent to the intermediate resin is (3-10):1, and the solvent is at least one of toluene, xylene, methylal, acetone and ethyl acetate.
The crosslinking degree of the resin spheres obtained in the step S1 is 10-80%, and the particle size of the resin spheres is 0.1-2.0 mm.
The mass to volume (g/mL) ratio of the resin beads to the organic carbon source in the step S2 is (2-5): (3-10), the mass concentration of the organic carbon source is 10-30%, and the rate of column adsorption is 0.5-20 BV/h.
In the high-pressure hydrothermal reaction in step S3, the volume ratio of the resin beads with the adsorbed organic carbon source to distilled water is 1: (1-5), the temperature of the high-pressure hydrothermal reaction is 120-180 ℃, the time is 2-20h, and the pressure is 0.2-0.8 MPa.
The mass concentration of the organic carbon source is preferably 10-15%, the rate of column adsorption is preferably 0.5-2BV/h, and the time of the high-pressure hydrothermal reaction is preferably 8-10 h.
A macroporous adsorbent resin is prepared by the above preparation method.
Compared with the prior art, the preparation method comprises the steps of performing synthesis extraction on an oil phase and a water phase mixed with a monomer, a cross-linking agent and a pore-foaming agent by using a suspension polymerization method to obtain resin spheres, adsorbing an organic carbon source to the resin spheres through a column by means of a stable skeleton of the resin spheres, and carrying active carbon on the resin skeleton after high-pressure hydrothermal reaction, so that the adsorption selectivity of the prepared macroporous adsorption resin is improved, and the performance of the macroporous adsorption resin is improved.
Detailed Description
The invention is further illustrated by the following specific examples.
The preparation method comprises the following steps:
s1, mixing a monomer, a cross-linking agent and a pore-foaming agent to obtain an oil phase, adding a water phase into a container, heating, adding the oil phase into the water phase, synthesizing by a suspension polymerization method, and extracting by using a solvent to obtain resin spheres with the cross-linking degree of 10-80% and the particle size of 0.1-2.0 mm;
the monomer comprises at least one of styrene, methyl acrylate and acrylonitrile, the cross-linking agent comprises divinylbenzene, the pore-foaming agent comprises at least one of white oil, liquid paraffin, solid paraffin, polystyrene and polymethyl acrylate, and the water phase comprises distilled water; the oil phase comprises 1-10 parts of monomer, 1-10 parts of cross-linking agent and 2-5 parts of pore-foaming agent by weight, and the water phase is 20-30 parts;
and S1, adding the water phase into a container, heating to 45-55 ℃, then uniformly mixing the oil phase, adding the oil phase into the water phase, heating to 65-75 ℃ for reaction for 3-8h, continuing heating to 85-95 ℃ for reaction for 3-10h, cooling to obtain intermediate resin, finally extracting the intermediate resin with a solvent, and after extraction, sequentially washing with distilled water at 90 ℃ or higher, boiling with water and drying to obtain the resin spheres. During extraction, the volume ratio of a solvent to the intermediate resin is (3-10) to 1, and the solvent is at least one of toluene, xylene, methylal, acetone and ethyl acetate;
s2, allowing the resin balls to pass through a column to adsorb an organic carbon source, wherein the organic carbon source is at least one of a sucrose solution, a glucose solution, a fructose solution, a galactose solution, a lactose solution and a maltose solution; the mass to volume (g/mL) ratio of the resin spheres to the organic carbon source was: (2-5): (3-10), wherein the mass concentration of the organic carbon source is 10-30%, the adsorption rate of the column chromatography is 0.5-20BV/h, the mass concentration of the organic carbon source is preferably 10-15%, and the adsorption rate of the column chromatography is preferably 0.5-2 BV/h;
s3, adding the resin balls adsorbed with the organic carbon source into distilled water for high-pressure hydrothermal reaction to obtain the macroporous adsorption resin loaded with the activated carbon, wherein in the high-pressure hydrothermal reaction, the volume ratio of the resin balls adsorbed with the organic carbon source to the distilled water is 1: (1-5), the temperature of the high-pressure hydrothermal reaction is 120-180 ℃, the time is 8-20h, preferably 8-10h, and the pressure is 0.2-0.8 MPa.
Example 1:
1) preparation of resin pellets
The formula comprises the following components in parts by weight:
adding the water phase into a 2000ml reaction kettle, heating to 55 ℃, uniformly mixing the oil phase, adding into the reaction kettle, controlling the particle size to be 0.3-1.0, heating to 75 ℃, continuing to heat to 90 ℃ after reacting for 3 hours, reacting for 5 hours, stopping the reaction, cooling to obtain an intermediate resin ball, washing with hot water at the temperature of more than 90 ℃, extracting with methylal with the volume of 5 times that of the intermediate resin ball, washing, decocting with water, and drying to obtain a product resin ball;
2) resin column
Taking 70g of the resin balls and loading the resin balls into an adsorption resin column for later use; preparing 300ml of 10% sucrose solution; allowing the sucrose solution to pass through a column, and allowing the resin balls to fully adsorb the sucrose solution; taking out the column after the column passing is finished for later use;
3) high pressure hydrothermal reaction
And (3) transferring the resin balls in the step 2) into a high-pressure reaction kettle, heating to 125 ℃, reacting for 8 hours, discharging, filtering and washing to obtain 78g of macroporous adsorption resin loaded with activated carbon.
Example 2:
1) preparation of resin pellets
The formula comprises the following components in parts by weight:
oil phase:
adding the water phase into a 2000ml reaction kettle, heating to 55 ℃, uniformly mixing the oil phase, adding into the reaction kettle, controlling the particle size to be 0.3-1.0, heating to 75 ℃, continuing to heat to 90 ℃ after reacting for 3 hours, reacting for 5 hours, stopping the reaction, cooling to obtain an intermediate resin ball, washing with hot water at the temperature of more than 90 ℃, extracting with toluene with the volume of 5 times that of the intermediate resin ball, washing, boiling with water, and drying to obtain a product resin ball;
2) resin column
Taking 70g of the resin balls and loading the resin balls into an adsorption resin column for later use; preparing 300ml of 12% sucrose solution; allowing the sucrose solution to pass through a column, and allowing the resin to fully adsorb the sucrose solution; taking out the column after the column passing is finished for later use;
3) high pressure hydrothermal reaction
And (3) transferring the resin balls in the step 2) into a high-pressure reaction kettle, heating to 135 ℃, reacting for 10 hours, discharging, filtering and washing to obtain 80g of macroporous adsorption resin loaded with activated carbon.
Example 3:
1) preparation of resin pellets
The formula comprises the following components in parts by weight:
adding the water phase into a 2000ml reaction kettle, heating to 55 ℃, uniformly mixing the oil phase, adding into the reaction kettle, controlling the particle size to be 0.3-1.0, heating to 75 ℃, continuing to heat to 90 ℃ after reacting for 3 hours, reacting for 5 hours, stopping the reaction, cooling to obtain an intermediate resin ball, washing with hot water at the temperature of more than 90 ℃, extracting with toluene with the volume of 5 times that of the intermediate resin ball, washing, boiling with water, and drying to obtain a product resin ball;
2) resin column
Taking 70g of the resin balls and loading the resin balls into an adsorption resin column for later use; preparing 300ml of 15% sucrose solution; allowing the sucrose solution to pass through a column, and allowing the resin balls to fully adsorb the sucrose solution; taking out the column after the column passing is finished for later use;
3) high pressure hydrothermal reaction
And (3) transferring the resin balls in the step 2) into a high-pressure reaction kettle, heating to 135 ℃, reacting for 10 hours, discharging, filtering and washing to obtain 74g of macroporous adsorption resin loaded with activated carbon.
Example 4:
1) preparation of resin pellets
The formula comprises the following components in parts by weight:
adding the water phase into a 2000ml reaction kettle, heating to 55 ℃, uniformly mixing the oil phase, adding into the reaction kettle, controlling the particle size to be 0.3-1.0, heating to 75 ℃, continuing to heat to 90 ℃ after reacting for 3 hours, reacting for 5 hours, stopping the reaction, cooling to obtain an intermediate resin ball, washing with hot water at the temperature of more than 90 ℃, extracting with toluene with the volume of 5 times that of the intermediate resin ball, washing, boiling with water, and drying to obtain a product resin ball;
2) resin column
Taking 70g of the resin balls and loading the resin balls into an adsorption resin column for later use; preparing 300ml of 12% fructose solution; allowing the sucrose solution to pass through a column, and allowing the resin balls to fully adsorb the fructose solution; taking out the column after the column passing is finished for later use;
3) high pressure hydrothermal reaction
Transferring the resin balls in the step 2) into a high-pressure reaction kettle, heating to 135 ℃, reacting for 10 hours, discharging, filtering and washing to obtain 85g of macroporous adsorption resin loaded with activated carbon.
Example 5:
1) preparation of resin pellets
The formula comprises the following components in parts by weight:
adding the water phase into a 2000ml reaction kettle, heating to 55 ℃, uniformly mixing the oil phase, adding into the reaction kettle, controlling the particle size to be 0.3-1.0, heating to 75 ℃, continuing to heat to 90 ℃ after reacting for 3 hours, reacting for 5 hours, stopping the reaction, cooling to obtain an intermediate resin ball, washing with hot water at the temperature of more than 90 ℃, extracting with toluene with the volume of 5 times that of the intermediate resin ball, washing, boiling with water, and drying to obtain a product resin ball;
2) resin column
Taking 70g of the resin balls and loading the resin balls into an adsorption resin column for later use; preparing 300ml of 12% lactose solution; passing the sucrose solution through a column to allow the resin to fully adsorb the lactose solution; taking out the column after the column passing is finished for later use;
3) high pressure hydrothermal reaction
And (3) transferring the resin balls in the step 2) into a high-pressure reaction kettle, heating to 145 ℃, reacting for 20 hours, discharging, filtering and washing to obtain 84g of macroporous adsorption resin loaded with activated carbon.
The macroporous adsorption resin obtained by the embodiment is loaded with the activated carbon, so that the adsorption selectivity of the macroporous adsorption resin is improved, and the adsorption of the macroporous adsorption resin on small molecular substances such as methanol and acetone is improved by more than 20%.
According to the invention, by means of the stable framework of the resin, the organic carbon source is subjected to column adsorption and high-pressure hydrothermal reaction, and then the activated carbon is loaded on the resin framework, so that the adsorption selectivity of the prepared macroporous adsorption resin is improved, and the performance of the macroporous adsorption resin is improved.
Claims (7)
1. A preparation method of macroporous adsorption resin loaded with activated carbon is characterized by comprising the following steps:
s1, mixing a monomer, a cross-linking agent and a pore-foaming agent to obtain an oil phase, adding a water phase into a container, heating, adding the oil phase into the water phase, synthesizing by a suspension polymerization method, and extracting by a solvent to obtain resin balls with the cross-linking degree of 10-80% and the particle size of 0.1-2.0 mm; the oil phase comprises, by mass, 1-10 parts of a monomer, 1-10 parts of a cross-linking agent and 2-5 parts of a pore-foaming agent, and the water phase is 20-30 parts; the monomer comprises at least one of styrene, methyl acrylate and acrylonitrile, the cross-linking agent comprises divinylbenzene, the pore-forming agent comprises at least one of white oil, liquid paraffin, solid paraffin, polystyrene and polymethyl acrylate, and the aqueous phase comprises distilled water;
s2, allowing the resin balls to pass through a column to adsorb an organic carbon source, wherein the organic carbon source is at least one of a sucrose solution, a glucose solution, a fructose solution, a galactose solution, a lactose solution and a maltose solution;
and S3, adding the resin balls adsorbed with the organic carbon source into distilled water to perform high-pressure hydrothermal reaction, and obtaining the active carbon loaded macroporous adsorption resin.
2. The preparation method according to claim 1, wherein the aqueous phase in step S1 is added into a container and heated to 45-55 ℃, then the oil phase is mixed and added into the aqueous phase and heated to 65-75 ℃ to react for 3-8h, then the mixture is heated to 85-95 ℃ to react for 3-10h and then cooled to obtain the intermediate resin, finally the intermediate resin is extracted by a solvent, and after extraction, the resin spheres are obtained by washing, boiling and drying with distilled water at 90 ℃ or higher in sequence.
3. The method according to claim 2, wherein in the step S1, when the solvent is used for extraction of the intermediate resin, the volume ratio of the solvent to the intermediate resin is (3-10):1, and the solvent is at least one of toluene, xylene, methylal, acetone, and ethyl acetate.
4. The method according to claim 1, wherein the mass-to-volume (g/mL) ratio of the resin beads to the organic carbon source in step S2 is (2-5): (3-10), the mass concentration of the organic carbon source is 10-30%, and the rate of column adsorption is 0.5-20 BV/h.
5. The method according to claim 4, wherein in the hydrothermal reaction at a high pressure in step S3, the volume ratio of the resin beads having the organic carbon source adsorbed thereon to distilled water is 1: (1-5), the temperature of the high-pressure hydrothermal reaction is 120-180 ℃, the time is 2-20h, and the pressure is 0.2-0.8 MPa.
6. The preparation method according to claim 5, wherein the mass concentration of the organic carbon source is preferably 10-15%, the rate of column adsorption is preferably 0.5-2BV/h, and the time of the high-pressure hydrothermal reaction is preferably 8-10 h.
7. A macroporous adsorbent resin obtained by the production method according to any one of claims 1 to 6.
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