CN113956385B - Preparation method of polymer binder formed by extrusion of activated carbon powder - Google Patents
Preparation method of polymer binder formed by extrusion of activated carbon powder Download PDFInfo
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- CN113956385B CN113956385B CN202111495095.5A CN202111495095A CN113956385B CN 113956385 B CN113956385 B CN 113956385B CN 202111495095 A CN202111495095 A CN 202111495095A CN 113956385 B CN113956385 B CN 113956385B
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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
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- 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
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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
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/18—Suspension polymerisation
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- 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
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Water Treatment By Sorption (AREA)
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Abstract
The invention discloses a preparation method of an active carbon powder extrusion molding polymer binder, which comprises the following steps: step 1, taking 100 parts of styrene, 0-6 parts of N-methylol acrylamide, 0-4 parts of itaconic acid, 3 parts of initiator and 10 parts of cosolvent, and uniformly mixing and stirring to form an oil phase; step 2, mixing 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 and the oil phase solution, and reacting for 5-10 hours at the temperature of 40-60 ℃ under the mechanical stirring action of 200-500 rpm; and step 4, after the reaction is finished, collecting solid powder in the reaction liquid, washing the solid powder with distilled water, and finally, vacuum drying the solid powder to obtain the adhesive 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, has simple flow and mild reaction conditions, and is suitable for large-scale industrial production.
Description
Technical Field
The invention relates to a preparation method of an active carbon powder extrusion molding polymer binder, belonging to the field of high polymer materials.
Background
The active carbon is prepared by using charcoal, various shells and high-quality coal as raw materials, screening, crushing, sieving, rinsing, drying, and activating by physical method (such as treating with air, carbon dioxide, steam, etc.) and chemical method (such as treating with phosphoric acid, potassium hydroxide, zinc chloride, etc.), so as to erode its surface and generate numerous fine pores to form a large number of micropore structures with diameters of about 2-50 nm, so that the active carbon has huge specific surface area (generally about 500-1500m 2 And/g), thereby exhibiting the effects of decoloring, deodorizing, filtering, adsorbing, purifying, catalyzing, etc. At present, the 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 great field of application for activated carbon is water purification. The active 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. In particular to a household water purifier, one of the core components is an active carbon filter core, and the household water purifier has the advantages of large specific surface area, adjustable aperture, integration of adsorption and interception, small secondary pollution, convenient use and replacement, low cost and the like. The active carbon filter core product mainly comprises a compressed active carbon filter core and a bulk active carbon filter core, and the compressed active carbon filter core is mainly used in the water purifier. The compression active carbon filter core forming process comprises the following steps: mixing active carbon powder with certain particle size and binding component (such as asphalt, coal tar, starch, cooked rubber powder, etc.) with certain proportion, compression molding, and sintering and carbonizing at high temperature to obtain the filter element. The filter element obtained by the sintering process has the defects of lower 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, an activated carbon filter element extrusion molding process is becoming the mainstream. The extrusion molding of the active carbon filter element requires the use of polymer binder powder with a certain proportion, the polymer binder powder and the active 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 form the filter element. In order to ensure the quality of household drinking water, the polymer binder used needs to have enough stability and hydrolysis resistance, is nontoxic and sanitary, does not contain heavy metals and other easy-to-spill small molecules so as to prevent the pollution of the drinking water, and is mainly Polyethylene (PE) powder in the market at present. Compared with the sintering molding process of the active carbon filter element, the extrusion molding has the advantages of low processing temperature of the filter element, low energy consumption, simple process, rapid molding, high production efficiency, no waste gas pollution and the like. However, as 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 formed filter element has lower tensile strength, the filter element is easy to break, the polyethylene usage amount is larger, the cost is higher, and the water filtering flow of the filter element is reduced and the purifying capacity is reduced due to the nonpolar polyethylene polymer in the filter element.
Disclosure of Invention
Aiming at the defects of a polyethylene powder binder in the existing active carbon extrusion molding process, the invention provides a preparation method of a polymer binder which can bond active carbon powder and can be extruded, and the binder can improve the bonding performance of the active carbon powder and enhance the tensile strength of an active carbon filter element; meanwhile, the adhesive powder is produced by using a suspension polymerization process, has simple flow and mild reaction conditions, and is suitable for large-scale industrial production.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the preparation method of the polymer binder extruded by the activated carbon powder comprises the following steps:
step 1, taking 100 parts of styrene, 0-6 parts of N-methylol 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 and 20 parts of sodium chloride, and uniformly stirring and mixing to prepare a water phase;
step 3, introducing nitrogen into the reactor to remove oxygen, adding the water phase and the oil phase solution, and reacting for 5-10 hours 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, vacuum drying the solid powder to obtain the binder powder;
the parts are weight parts.
Preferably, the initiator in the step 1 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 component proportion can further increase the water purifying capacity of the active carbon filter element.
Preferably, the reaction temperature in step 3 is 50 ℃.
Preferably, in step 3, the stirring rate is 300rpm.
Preferably, the reaction time in step 3 is 8h.
As a further preference, the reaction temperature in step 3 is 50℃and 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 molding binder, which uses styrene as a main monomer, and through suspension copolymerization with N-methylol acrylamide and itaconic acid monomer, not only can the polarity of a styrene copolymer be improved, and the binding property of the copolymer to the active carbon powder be increased, but also the hydrophilic property of an active carbon filter element can be improved, so that the permeability coefficient of the active carbon filter element to water can be increased, and the water purifying flow and the water purifying efficiency of the active carbon filter element can be improved. Compared with a nonpolar polyethylene binder, the styrene copolymer binder provided by the invention has higher bonding strength and higher water purification efficiency under the condition of proper formula composition. The adhesive powder is produced by using a suspension polymerization process, has simple flow and mild reaction conditions, and is suitable for large-scale industrial production.
Detailed Description
The invention will now be further described with reference to examples. The described embodiments are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The specific implementation method of the active carbon powder extrusion molding binder provided by the invention comprises the following steps: 100 parts of styrene, 2-8 parts of N-methylolacrylamide, 0-5 parts of itaconic acid, 3 parts of azodiisoheptonitrile and 10 parts of methanol are taken according to parts by weight and stirred and mixed uniformly to form an oil phase; then, 400 parts of distilled water, 2 parts of polyvinyl alcohol 1788 and 20 parts of sodium chloride are stirred and mixed uniformly to prepare a water phase; introducing nitrogen into the reactor to remove oxygen, adding the aqueous phase and the oil phase solution, and reacting for 6-10h at 40-60 ℃ under the mechanical stirring action of 200-500 rpm; after the reaction is finished, collecting solid powder in the reaction liquid, washing the solid powder with distilled water, and finally, vacuum drying the solid powder to obtain the binder powder.
Characterization test method for activated carbon filter element
Preparing an activated carbon filter element sample strip: the polymer binder powder is sieved, powder between 100 and 200 meshes is reserved, the powder is mixed with a certain amount of activated carbon powder (coconut shell powder activated carbon, jiangsu Pu Shida and 100 to 200 meshes) according to a proportion, and the mixed powder is added into an extruding machine and is extruded into a die to be molded to obtain a test bar. The test bars were tested for breaking strength on a WDT-20KN electronic all-purpose material testing machine.
And (3) measuring the tensile strength of the activated carbon filter element: tensile strength σ=p/(b×d) of the activated carbon filter element. Wherein sigma is the tensile strength or breaking strength of the filter element, P is the maximum breaking load (N) at two ends of the experiment, b is the width of the test strip, and d is the thickness of the test strip. The breaking strength of the activated carbon filter element was determined by the method of GB/T1040-1992.
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 (cm 3) of the activated carbon filter element
And (3) measuring the permeability coefficient of the activated carbon filter element: the permeability coefficient K=QLρg/ΔpA of water in the active carbon filter element, 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, ρ is the water density, g is the gravity acceleration, Δp is the liquid level pressure difference at two ends of the filter element, and A is the cross section area of the filter element. The determination was carried out according to the industry standard MT 224-1990.
Activated carbon filter core water purification flow: the flow rate of purified water per unit time to the activated carbon filter cartridge is calculated according to the size (length×outer diameter×inner diameter=250×62×40 mm) of the activated carbon filter cartridge of a general household water purifier.
Example 1
The specific synthetic method steps of the activated carbon powder forming binder and the activated carbon filter element characterization test method described in example 1 are shown in the above specific embodiments and the activated carbon filter element characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 0.3g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 300rpm. Reaction temperature: 50 ℃; the reaction time was 8h. Activated carbon powder and binderThe mass ratio of the powder is 7:3. The density of the prepared activated carbon filter element is 0.481g/cm 3 The tensile strength was 8.36kPa. Permeability coefficient: 0.181cm/s. The flow rate of the purified water is 5.30L/min.
Example 2
The specific synthetic method steps of the activated carbon powder forming binder and the activated carbon filter characterization test method described in example 2 are shown in the above specific embodiments and the activated carbon filter characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 1.5g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 300rpm. Reaction temperature: 40 ℃; the reaction time was 10h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.484g/cm 3 The tensile strength was 10.6kPa. Permeability coefficient: 0.117cm/s. The flow rate of the purified water is 3.42L/min.
Example 3
The specific synthetic method steps and the activated carbon filter element characterization test method of the activated carbon powder forming binder described in example 3 are shown in the above specific embodiments and the activated carbon filter element characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 0.5g of N-methylolacrylamide, 0g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 200rpm. Reaction temperature: 60 ℃; the reaction time was 6h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.483g/cm 3 The tensile strength was 19.6kPa. Permeability coefficient: 0.089cm/s. The flow rate of the purified water is 2.60L/min.
Example 4
The specific synthetic method steps and the activated carbon filter characterization test method of the activated carbon powder forming binder described in example 4 are shown in the above specific embodiments and the activated carbon filter characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 0g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. Original water phaseThe material composition is as follows: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 400rpm. Reaction temperature: 50 ℃; the reaction time was 8h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.477g/cm 3 The tensile strength was 8.08kPa. Permeability coefficient: 0.078cm/s. The flow rate of the purified water was 2.27L/min.
Example 5
The specific synthetic method steps of the activated carbon powder forming binder and the activated carbon filter characterization test method described in example 5 are shown in the above specific embodiments and the activated carbon filter characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 1.0g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 400rpm. Reaction temperature: 60 ℃; the reaction time was 8h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.479g/cm 3 The tensile strength was 10.1kPa. Permeability coefficient: 0.158cm/s. The flow rate of the purified water was 4.63L/min.
Example 6
The specific synthetic method steps of the activated carbon powder forming binder and the activated carbon filter characterization test method described in example 6 are shown in the above specific embodiments and the activated carbon filter characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 0.5g of N-methylolacrylamide, 0.5g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 500rpm. Reaction temperature: 50 ℃; the reaction time was 8h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.478g/cm 3 The tensile strength was 6.5kPa. Permeability coefficient: 0.110cm/s. The flow rate of the purified water is 3.23L/min.
Example 7
Specific synthetic method steps and activated carbon filter characterization test method of activated carbon powder forming binder described in example 7 are as described in the above detailed description and activated carbon filter characterization testThe method is shown. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 1.5g of N-methylolacrylamide, 0g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 300rpm. Reaction temperature: 50 ℃; the reaction time was 8h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.482g/cm 3 The tensile strength was 21.6kPa. Permeability coefficient: 0.078cm/s. The flow rate of the purified water was 2.27L/min.
Example 8
The specific synthetic method steps and the activated carbon filter characterization test method of the activated carbon powder forming binder described in example 8 are shown in the above specific embodiments and the activated carbon filter characterization test method. Wherein the oil phase raw materials comprise the following components: 25g of styrene, 0g of N-methylolacrylamide, 1.0g of itaconic acid, 0.6g of azodiisoheptonitrile and 2.5g of methanol. The water phase raw materials comprise the following components: 100g of water, 1788.5 g of polyvinyl alcohol and 5g of sodium chloride. Stirring rotation speed: 400rpm. Reaction temperature: 50 ℃; the reaction time was 8h. The mass ratio of the activated carbon powder to the binder powder is 7:3. The density of the prepared active carbon filter element is 0.480g/cm 3 The tensile strength was 8.74kPa. Permeability coefficient: 0.124cm/s. The flow rate of the purified water was 3.62L/min.
Example 9 (comparative example)
Example 9 is a comparative example. Example 9 an activated carbon filter cartridge was prepared under the same conditions using a commercially available ultra high molecular weight PE powder (medium plasticization, molecular weight 500 ten thousand, particle size 100/200 mesh) binder for comparison. The mass ratio of the active carbon powder to the PE binder powder is 7:3. The density of the prepared active carbon filter element is 0.489g/cm 3 The tensile strength was 3.42kPa. Permeability coefficient: 0.179cm/s. The flow rate of the purified water is 5.24L/min.
Claims (6)
1. A preparation method of an active carbon powder extrusion molding polymer binder is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1, taking 100 parts of styrene, 0.3-1.5 parts of N-methylol acrylamide, 0.5-1.0 parts of itaconic acid, 3 parts of initiator and 10 parts of cosolvent, and uniformly mixing and stirring to form an oil phase;
step 2, mixing 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 and the oil phase solution, and reacting at 40-60 ℃ for 5-10h 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, vacuum drying the solid powder to obtain the binder powder;
the parts are weight parts.
2. The method of claim 1, wherein: the initiator in the step 1 is azo-diisoheptonitrile, and the cosolvent is methanol.
3. The method of claim 2, wherein: the reaction temperature in step 1 was 50 ℃.
4. The method of claim 2, wherein: the stirring rate in step 1 was 300rpm.
5. The method of claim 2, wherein: the reaction time in step 1 was 8h.
6. The method of claim 2, wherein: the reaction temperature in step 3 was 50℃and 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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