CN113956385A - Preparation method of activated carbon powder extrusion molding polymer binder - Google Patents
Preparation method of activated carbon powder extrusion molding polymer binder Download PDFInfo
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- CN113956385A CN113956385A CN202111495095.5A CN202111495095A CN113956385A CN 113956385 A CN113956385 A CN 113956385A CN 202111495095 A CN202111495095 A CN 202111495095A CN 113956385 A CN113956385 A CN 113956385A
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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
- C08F212/02—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/08—Special characteristics of binders
- B01D2239/086—Binders between particles or fibres
Abstract
The invention discloses a preparation method of an activated carbon powder extrusion molding polymer binder, which comprises the following steps: step 1, mixing and stirring 100 parts of styrene, 0-6 parts of N-hydroxymethyl acrylamide, 0-4 parts of itaconic acid, 3 parts of initiator and 10 parts of cosolvent uniformly to form an oil phase; step 2, mixing and stirring 400 parts of distilled water, 2 parts of polyvinyl alcohol 1788 and 20 parts of sodium chloride uniformly to prepare a water phase; step 3, introducing nitrogen into the reactor to remove oxygen, adding the water phase solution and the oil phase solution, and reacting for 5-10h at the temperature of 40-60 ℃ under the mechanical stirring action of 200-500 rpm; and 4, after the reaction is finished, collecting solid powder in the reaction liquid, washing the solid powder by using distilled water, and finally drying the solid powder in vacuum to obtain the binder powder. The adhesive can improve the adhesive property of the activated carbon powder and enhance the tensile strength of the activated carbon filter element; meanwhile, the adhesive powder is produced by using a suspension polymerization process, the process is simple, the reaction conditions are mild, and the method is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a preparation method of an activated carbon powder extrusion molding polymer binder, belonging to the field of high polymer materials.
Background
The activated carbon is prepared by taking charcoal, various shells, high-quality coal and the like as raw materials, screening, crushing, sieving, rinsing and drying the raw materials, and activating the raw materials by a physical method (such as treatment by air, carbon dioxide, water vapor and the like under a heating condition) and a chemical method (such as treatment by phosphoric acid, potassium hydroxide, zinc chloride and the like) to corrode the surface of the raw materials to generate countless fine pores and form a large number of microporous structures with the diameter of about 2-50 nm, so that the activated carbon has a huge specific surface area (generally about 500-1500 m)2/g) so as to exert the functions of decoloring, deodorizing, filtering, adsorbing, purifying, catalyzing and the like. Currently, activated carbon is widely applied to the fields of chemical industry, medicine, environment, energy, electronics, bioengineering, life science and the like as an industrial adsorbent.
A large field of application of activated carbon is water purification. The activated carbon can remove chlorine, colloid, organic matters and heavy metals in water, and is the earliest and most widely used water purifying material in the water purifier. Particularly, in the household water purifier, one of the core components is an active carbon filter element, and the active carbon filter element has the advantages of large specific surface area, adjustable pore diameter, integration of adsorption and interception, small secondary pollution, convenient use and replacement, low cost and the like. The active carbon filter element product mainly comprises a compressed active carbon filter element and a bulk active carbon filter element, and the compressed active carbon filter element is mainly used in the water purifier. The forming process of the compressed activated carbon filter element comprises the following steps: the active carbon powder with a certain particle size and a certain proportion of bonding components (such as asphalt, coal tar, starch, cooked rubber powder and the like) are uniformly mixed, compressed and molded, and then sintered and carbonized at high temperature to prepare the filter element. The filter element obtained by the sintering process has the defects of low bonding strength, overhigh processing temperature, high energy consumption, complex process, serious pollution and the like.
In recent years, in the field of household water purifiers, the extrusion molding process of the activated carbon filter element is becoming mainstream. The extrusion molding of the activated carbon filter element needs to use a certain proportion of polymer binder powder, the polymer binder powder and the activated carbon powder with a certain particle size are uniformly mixed in an extruding machine, and then the mixture is extruded into a die at a certain temperature and pressure to be molded to obtain the filter element. In order to ensure the quality of household drinking water, the polymer binder needs to have sufficient stability and hydrolysis resistance, is nontoxic and sanitary, does not contain heavy metals and other easily-leaked small molecules so as to prevent the drinking water from being polluted, and the polymer binder mainly comprises Polyethylene (PE) powder. Compared with the sintering forming process of the activated carbon filter element, the extrusion forming process has the advantages of low processing temperature of the filter element, less energy consumption, simple process, quick forming, high production efficiency, no waste gas pollution and the like. However, because the surface of the activated carbon contains a plurality of polar groups (such as hydroxyl, carboxyl, carbonyl and the like), the compatibility of the nonpolar polyethylene polymer to the polar groups is poor, so that the bonding performance of the polyethylene to the activated carbon powder is poor, the tensile strength of the formed filter element is low, the filter element is easy to break, the polyethylene consumption is large, the cost is high, and the nonpolar polyethylene polymer in the filter element also reduces the filtered water flow of the filter element and the purification capacity.
Disclosure of Invention
Aiming at the defects of polyethylene powder binder in the existing activated carbon extrusion forming process, the invention provides a preparation method of polymer binder capable of binding activated carbon powder and carrying out extrusion forming, the binder can improve the binding property of the activated carbon powder and enhance the tensile strength of an activated carbon filter element; meanwhile, the adhesive powder is produced by using a suspension polymerization process, the process is simple, the reaction conditions are mild, and the method is suitable for large-scale industrial production.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of an activated carbon powder extrusion molding polymer binder comprises the following steps:
step 1, taking 100 parts of styrene, 0-6 parts of N-hydroxymethyl acrylamide, 0-4 parts of itaconic acid, 3 parts of initiator and 10 parts of cosolvent, and stirring and mixing uniformly to form an oil phase;
step 2, taking 400 parts of distilled water, 2 parts of polyvinyl alcohol 1788 type and 20 parts of sodium chloride, stirring and mixing uniformly to prepare a water phase;
step 3, introducing nitrogen into the reactor to remove oxygen, adding the water phase solution and the oil phase solution, and reacting for 5-10h at the temperature of 40-60 ℃ under the mechanical stirring action of 200-500 rpm;
step 4, after the reaction is finished, collecting solid powder in the reaction liquid, washing the solid powder with distilled water, and finally drying the solid powder in vacuum to obtain the binder powder;
the parts are all parts by weight.
Preferably, in the step 1, the initiator is azobisisoheptonitrile, and the cosolvent is methanol.
Preferably, in step 1, 100 parts of styrene, 1.2 parts of N-methylolacrylamide, 2 parts of itaconic acid, 2.4 parts of azobisisoheptonitrile and 10 parts of methanol are taken. The proportion of the components can further increase the water purifying capacity of the activated carbon filter element.
Preferably, the reaction temperature in step 3 is 50 ℃.
Preferably, in step 3, the stirring rate is 300 rpm.
Preferably, the reaction time in step 3 is 8 h.
As a further preference, the reaction temperature in step 3 is 50 ℃, the stirring rate is 300rpm, and the reaction time is 8 hours.
Compared with the prior art, the invention has the beneficial effects that: the invention provides a preparation method of an active carbon powder extrusion forming binder, which takes styrene as a main monomer, and carries out suspension copolymerization with N-hydroxymethyl acrylamide and itaconic acid monomers, so that the polarity of a styrene copolymer can be improved, the adhesive property of the copolymer to active carbon powder is increased, and the hydrophilic property of an active carbon filter element is improved, thereby increasing the permeability coefficient of the active carbon filter element to water, and improving the water purification flow and the water purification efficiency of the active carbon filter element. Compared with a non-polar polyethylene binder, the styrene copolymer binder provided by the invention has the advantages that the obtained extruded and formed activated carbon filter element has higher binding strength and higher water purification efficiency under the condition of proper formula composition. The invention has the advantages of simple process, mild reaction condition and suitability for large-scale industrial production.
Detailed Description
The invention will now be further described with reference to the following examples. The described embodiments are only some embodiments of the invention, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The specific implementation method of the activated carbon powder extrusion molding binder provided by the invention comprises the following steps: taking 100 parts by weight of styrene, 2-8 parts by weight of N-hydroxymethyl acrylamide, 0-5 parts by weight of itaconic acid, 3 parts by weight of azobisisoheptonitrile and 10 parts by weight of methanol, and stirring and mixing uniformly to form an oil phase; then, 400 parts of distilled water, 2 parts of polyvinyl alcohol 1788 type and 20 parts of sodium chloride are taken to be stirred and mixed evenly to prepare a water phase; introducing nitrogen into the reactor to remove oxygen, adding the water phase solution and the oil phase solution, and reacting for 6-10h at the temperature of 40-60 ℃ under the mechanical stirring action of 200-500 rpm; and after the reaction is finished, collecting solid powder in the reaction liquid, washing the solid powder with distilled water, and finally drying the solid powder in vacuum to obtain the binder powder.
Characterization test method for activated carbon filter element
Preparing an activated carbon filter element sample strip: sieving the polymer binder powder, reserving the powder of 100-200 meshes, uniformly mixing the powder with a certain amount of activated carbon powder (coconut shell powder activated carbon, Jiangsu Pushmada, 100-200 meshes) according to a proportion, adding the mixed powder into an extruding machine, and extruding into a die to mold to obtain a sample strip. The test specimens were tested for fracture strength on a WDT-20KN electronic universal material testing machine.
And (3) measuring the tensile strength of the activated carbon filter element: the tensile strength σ of the activated carbon filter element is P/(b × d). Wherein, sigma is the tensile strength or the breaking strength of filter core, P is the biggest breaking load (N) at experiment both ends, and b examination sample width, d are sample strip thickness. The breaking strength of the activated carbon filter element is determined by the method of GB/T1040-.
And (3) measuring the density of the activated carbon filter element: the density of the activated carbon filter element is equal to the mass (g) of the activated carbon filter element/the volume (cm3) of the activated carbon filter element
And (3) measuring the permeability coefficient of the activated carbon filter element: the permeability coefficient K of water in the activated carbon filter element is QL rho g/delta pA, wherein K is the permeability coefficient, Q is the water quantity passing through the filter element in unit time, L is the thickness of the filter element, rho is the density of water, g is the gravity acceleration, delta p is the liquid level pressure difference between two ends of the filter element, and A is the cross-sectional area of the filter element. The assay was performed according to the industry standard MT 224-1990.
The flow rate of purified water of the activated carbon filter element is as follows: the flow rate of purified water to the activated carbon filter element per unit time is calculated according to the size (length x outer diameter x inner diameter) of the activated carbon filter element of a general household water purifier and the permeability coefficient.
Example 1
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core in example 1 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 0.3g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 300 rpm. Reaction temperature: 50 ℃; the reaction time is 8 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.481g/cm3The tensile strength was 8.36 kPa. Permeability coefficient: 0.181 cm/s. The flow rate of the purified water is 5.30L/min.
Example 2
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core in example 2 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 1.5g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 300 rpm. Reaction temperature: 40 ℃; the reaction time is 10 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.484g/cm3The tensile strength was 10.6 kPa. Permeability coefficient: 0.117 cm/s. The flow rate of the purified water was 3.42L/min.
Example 3
Example 3 specific Synthesis procedure for activated carbon powder Molding Binder and activated carbon Filter characterization test methodsThe specific implementation mode and the characterization and test method of the activated carbon filter element are shown. Wherein the oil phase comprises the following raw materials: 25g of styrene, 0.5g of N-methylolacrylamide, 0g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 200 rpm. Reaction temperature: 60 ℃; the reaction time is 6 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.483g/cm3The tensile strength was 19.6 kPa. Permeability coefficient: 0.089 cm/s. The flow rate of the purified water is 2.60L/min.
Example 4
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core described in example 4 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 0g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 400 rpm. Reaction temperature: 50 ℃; the reaction time is 8 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.477g/cm3The tensile strength was 8.08 kPa. Permeability coefficient: 0.078 cm/s. The flow rate of the purified water was 2.27L/min.
Example 5
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core described in example 5 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 1.0g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 400 rpm. Reaction temperature: 60 ℃; the reaction time is 8 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.479g/cm3The tensile strength was 10.1 kPa. Permeability coefficient: 0.158 cm/s. The flow rate of the purified water is 4.63L/min.
Example 6
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core described in example 6 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 0.5g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 500 rpm. Reaction temperature: 50 ℃; the reaction time is 8 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.478g/cm3The tensile strength was 6.5 kPa. Permeability coefficient: 0.110 cm/s. The flow rate of the purified water is 3.23L/min.
Example 7
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core described in example 7 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 1.5g of N-methylolacrylamide, 0g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 300 rpm. Reaction temperature: 50 ℃; the reaction time is 8 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.482g/cm3The tensile strength was 21.6 kPa. Permeability coefficient: 0.078 cm/s. The flow rate of the purified water was 2.27L/min.
Example 8
The specific steps of the method for synthesizing the activated carbon powder forming binder and the characterization test method of the activated carbon filter core described in example 8 are shown in the above specific embodiments and the characterization test method of the activated carbon filter core. Wherein the oil phase comprises the following raw materials: 25g of styrene, 0g of N-methylolacrylamide, 1.0g of itaconic acid, 0.6g of azobisisoheptonitrile and 2.5g of methanol. The water phase raw material comprises the following components: 100g of water, 17880.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring speed: 400 rpm. Reaction temperature: 50 ℃; the reaction time is 8 h. The mass ratio of the activated carbon powder to the binder powder is 7: 3. Density of the prepared active carbon filter elementDegree of 0.480g/cm3The tensile strength was 8.74 kPa. Permeability coefficient: 0.124 cm/s. The flow rate of the purified water was 3.62L/min.
Example 9 (comparative example)
Example 9 is a comparative example. Example 9 a comparison was made of an activated carbon filter element using a commercially available ultra high molecular weight PE powder (medium plasticized, 500 ten thousand molecular weight, particle size 100/200 mesh) binder under the same conditions. The mass ratio of the activated carbon powder to the PE binder powder is 7: 3. The density of the prepared activated carbon filter element is 0.489g/cm3The tensile strength was 3.42 kPa. Permeability coefficient: 0.179 cm/s. The flow rate of the purified water is 5.24L/min.
Claims (7)
1. A preparation method of an activated carbon powder extrusion molding polymer binder is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1, mixing and stirring 100 parts of styrene, 0-6 parts of N-hydroxymethyl acrylamide, 0-4 parts of itaconic acid, 3 parts of initiator and 10 parts of cosolvent uniformly to form an oil phase;
step 2, mixing and stirring 400 parts of distilled water, 2 parts of polyvinyl alcohol 1788 and 20 parts of sodium chloride uniformly to prepare a water phase;
step 3, introducing nitrogen into the reactor to remove oxygen, adding the water phase solution and the oil phase solution, and reacting for 5-10h at the temperature of 40-60 ℃ under the mechanical stirring action of 200-500 rpm;
step 4, after the reaction is finished, collecting solid powder in the reaction liquid, washing the solid powder with distilled water, and finally drying the solid powder in vacuum to obtain the binder powder;
the parts are all parts by weight.
2. The method of claim 1, wherein: in the step 1, 100 parts of styrene, 1.2 parts of N-methylolacrylamide, 2 parts of itaconic acid, 2.4 parts of azobisisoheptonitrile and 10 parts of methanol are taken.
3. The production method according to claim 1 or 2, characterized in that: in the step 1, the initiator is azobisisoheptonitrile, and the cosolvent is methanol.
4. The method of claim 3, wherein: the reaction temperature in step 1 was 50 ℃.
5. The method of claim 3, wherein: the stirring rate in step 1 was 300 rpm.
6. The method of claim 3, wherein: the reaction time in step 1 was 8 h.
7. The method of claim 3, wherein: the reaction temperature in step 3 was 50 ℃, the stirring rate was 300rpm, and the reaction time was 8 hours.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11158204A (en) * | 1997-11-26 | 1999-06-15 | Mitsui Chem Inc | Suspension polymerization |
| CN101400755A (en) * | 2006-03-08 | 2009-04-01 | 3M创新有限公司 | Pressure sensitive adhesive containing silica nanoparticles |
| KR20140110548A (en) * | 2013-03-08 | 2014-09-17 | 수산고분자 주식회사 | Compositions of thickener comprising natural oils |
| CN105916885A (en) * | 2014-01-17 | 2016-08-31 | 3M创新有限公司 | Self-wetting adhesive emulsion composition |
| CN115216255A (en) * | 2022-07-26 | 2022-10-21 | 珠海辰玉新材料科技有限公司 | Emulsion type binder, preparation method of emulsion type binder and diaphragm |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11158204A (en) * | 1997-11-26 | 1999-06-15 | Mitsui Chem Inc | Suspension polymerization |
| CN101400755A (en) * | 2006-03-08 | 2009-04-01 | 3M创新有限公司 | Pressure sensitive adhesive containing silica nanoparticles |
| KR20140110548A (en) * | 2013-03-08 | 2014-09-17 | 수산고분자 주식회사 | Compositions of thickener comprising natural oils |
| CN105916885A (en) * | 2014-01-17 | 2016-08-31 | 3M创新有限公司 | Self-wetting adhesive emulsion composition |
| CN115216255A (en) * | 2022-07-26 | 2022-10-21 | 珠海辰玉新材料科技有限公司 | Emulsion type binder, preparation method of emulsion type binder and diaphragm |
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