CN111467875A - Nano-cellulose glass fiber composite filter material and preparation method and application thereof - Google Patents
Nano-cellulose glass fiber composite filter material and preparation method and application thereof Download PDFInfo
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- CN111467875A CN111467875A CN202010347558.2A CN202010347558A CN111467875A CN 111467875 A CN111467875 A CN 111467875A CN 202010347558 A CN202010347558 A CN 202010347558A CN 111467875 A CN111467875 A CN 111467875A
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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
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H13/00—Pulp or paper, comprising synthetic cellulose or non-cellulose fibres or web-forming material
- D21H13/36—Inorganic fibres or flakes
- D21H13/38—Inorganic fibres or flakes siliceous
- D21H13/40—Inorganic fibres or flakes siliceous vitreous, e.g. mineral wool, glass fibres
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/10—Coatings without pigments
- D21H19/14—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
- D21H19/34—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising cellulose or derivatives thereof
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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
- B01D2239/10—Filtering material manufacturing
Abstract
The invention belongs to the field of filtration, and particularly relates to a nano-cellulose glass fiber composite filter material as well as a preparation method and application thereof. The method comprises the following steps: (1) defibering the fibrillatable plant fibers by a defibering machine, and dispersing in water to obtain slurry; (2) processing by a physical or chemical method to obtain nano-cellulose, washing, and performing ultrasonic treatment to obtain a nano-cellulose solution; (3) uniformly dispersing a glass fiber raw material with water and a dispersing agent to obtain slurry, and sequentially removing slag, diluting, forming and dehydrating to form wet paper pages with uniform thickness; (4) coating the surface of the glass fiber paper with the nano cellulose solution in a coating mode to form a nano fiber coating; (5) and (5) drying and forming. The nano cellulose solution prepared from the plant fibers is compounded with the glass fiber base material in a coating mode, so that the obtained filter material has the advantages of high precision, high air permeability, low resistance, long service life and the like, and is particularly suitable for the field of filtration of air, water and the like.
Description
Technical Field
The invention belongs to the field of filtration, and particularly relates to a nano-cellulose glass fiber composite filter material, and a preparation method and application thereof.
Background
Although conventional glass fiber filter materials can achieve effective filtration of contaminant particulates, the need to achieve higher filtration efficiencies often results in a sacrifice in air permeability and thus a greater pressure drop. Therefore, it is difficult to achieve an effective balance between the filtering efficiency and the pressure resistance by only the structural characteristics of the glass fiber itself.
In recent years, more and more researches are biased to prepare a composite filter material of nano fibers and glass fibers, so that the filter material has ultrahigh filtering precision on one hand, and the characteristic of deep filtration of the glass fibers on the other hand can be reserved. The existing methods for preparing the composite filter material of the nano fiber and the glass fiber mainly comprise the following two methods.
The first is an electrostatic spinning method, and patent CN105233568A discloses an electrostatic spinning method and a nanofiber/glass fiber composite filter material prepared by the method. The method forms a sandwich structure in which glass fiber filter paper and nano fibers with a electret effect are arranged alternately, and the nano fiber/glass fiber composite filter material is prepared. However, this method has the following problems: the adopted organic high molecular polymers such as polyacrylonitrile, polyvinylidene fluoride, polyurethane and the like also use a large amount of organic reagents such as tetrahydrofuran, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, acetone and the like in the spinning process, are not environment-friendly, have low electrostatic spinning efficiency, and are not suitable for industrial production and the like.
The other method is a slurry mixing method, and patent CN105937193A discloses a nano-sized air-filter paper and a preparation method thereof, wherein bamboo pulp, dracaena cochinchinensis pulp, softwood pulp, aramid fiber, carbon fiber, polyaryl oxadiazole fiber and glass fiber are added with water to prepare cellulose nanofiber slurry, the cellulose nanofiber slurry, a nano-cellulose crystal colloid, a fibrous binder, lignin, a dispersing agent, a defoaming agent and a waterproof agent are pulped to obtain pulp, the pulp is prepared into base paper, and then gum dipping is carried out to obtain the nano-sized air-filter paper. However, a large amount of chemicals are also added in the preparation process of the cellulose nanofiber prepared by the method, and in the process of pulping the cellulose nanofiber pulp and other substances to prepare pulp, the cellulose nanofiber pulp has the problems of difficult dispersion, flocculation and the like, so that the performance of the final product is poor.
Disclosure of Invention
The invention aims to provide a nano-cellulose glass fiber composite filter material, and a preparation method and application thereof.
The technical solution for realizing the purpose of the invention is as follows: a method for preparing a nano-cellulose glass fiber composite filter material specifically comprises the following steps:
step (1): preparing a nano cellulose solution;
step (2): preparing a wet glass fiber paper sheet;
and (3): coating the nano cellulose solution obtained in the step (1) on the surface of the glass fiber wet paper sheet obtained in the step (2) in a coating mode;
and (4): drying and forming to obtain the nano cellulose glass fiber composite filter material.
Further, the step (1) specifically includes:
step (1-1): soaking a plant fiber pulp board capable of fibrillating in water, defibering by a defibering machine, dispersing in water to obtain uniform fiber suspension, filtering, wringing, and balancing moisture for later use;
step (1-2): processing by physical or chemical method to obtain nano cellulose, washing, quantifying, and performing ultrasonic treatment to obtain nano cellulose solution.
Further, the plant fiber pulp board which can be fibrillated in the step (1-1) is one or more of softwood pulp, hardwood pulp, cotton pulp, hemp pulp, mercerized wood pulp, mercerized cotton pulp or mercerized hemp pulp.
Further, the pulp board soaking time in the step (1-1) is more than 4h, the rotational speed of the fluffer is 1000-.
Further, the chemical process is a TEMPO oxidation process.
Further, the concentration range of the nano-cellulose solution quantitatively obtained in the step (1-2) is 0.01% -3%.
Preferably, the cellulose concentration is 0.1% -1.5%;
the ultrasonic oscillation power is 200 + 10000KW, and the oscillation time is not less than 4h until a clear and uniform solution is obtained.
Further, the step (2) of preparing the glass fiber wet paper specifically comprises the following steps:
adding water and a dispersing agent into a glass fiber raw material, uniformly dispersing to obtain a slurry, and sequentially removing slag, diluting, forming and dehydrating to form a wet paper sheet with uniform thickness.
Further, the raw material of the glass fiber paper is preferably micro fiber cotton;
the dispersant is one or a mixture of more than two of a surfactant, a water-soluble high molecular compound or an acid.
Further, the surfactant is quaternary ammonium salt or fatty acid salt, and the acid is sulfuric acid, acetic acid or oxalic acid.
Further, the water-soluble high molecular compound is polyoxyethylene or polyacrylamide.
Further, in the step (2), the concentration of the slurry is 0.5-5%, the concentration after dilution is 0.1-1%, and the pH value of the slurry is 2-5.
Further, the thickness of the glass fiber paper web obtained in the step (2) is 0.1-0.5 mm;
the preferred web thickness is 0.25-0.35 mm.
Further, the coating mode in the step (3) is one of roll coating and knife coating;
and (4) drying in one or more of roller drying, infrared drying and hot air drying.
The nano-cellulose glass fiber composite filter material prepared by the method comprises a glass fiber base material and a nano-cellulose layer coated on the surface of the glass fiber base material.
The application of the nano-cellulose glass fiber composite filter material prepared by the method is used for filtering.
Further, for gas or liquid filtration
Compared with the prior art, the invention has the remarkable advantages that:
(1) the novel nano-cellulose/glass fiber composite filter material is obtained by compounding the nano-cellulose solution prepared from the plant fibers with the glass fiber base material in a coating mode, and has the advantages of high precision, high air permeability, low resistance, long service life and the like.
(2) The concentration of the nano-cellulose is dispersed more uniformly between 0.1 and 1.5. The sizing agent for the glass fiber adopts a cationic modifier, so that the surface of the glass fiber carries positive charges.
(3) The invention ensures the uniformity of the nano-cellulose by compounding in a coating mode; and the manufacturing process is simple, additional equipment is not required, and the method is suitable for large-scale production.
(4) In the preparation process of the invention, no chemical adhesive is used, the use of organic reagents is greatly reduced, and the invention has the advantages of environmental protection and no pollution.
(5) The nano-cellulose is prepared by a TEMPO oxidation method, a large amount of negative charges (carboxyl) carried by the TEMPO oxidized nano-cellulose and positive charges (amino) on the surface of glass fiber are combined by static electricity to form high-strength interlayer bonding force, and the problem of weak bonding strength between the nano-fiber and the glass fiber is effectively solved.
Detailed Description
The present invention is described in further detail below in conjunction with the following description.
A novel nano-cellulose/glass fiber composite filter material comprises a glass fiber base material and a nano-cellulose layer coated on the surface of the glass fiber base material.
The nanometer fiber/glass fiber composite material is used as gas filtering material and liquid filtering material.
A preparation method of a novel nano-cellulose/glass fiber composite filter material comprises the following steps:
(1) soaking the plant fiber pulp board capable of fibrillating in water for a certain time, defibering by a defibering machine, dispersing in water to obtain uniform fiber suspension, filtering, wringing, and balancing moisture for later use.
(2) Processing by a physical or chemical method to obtain nano-cellulose, washing, quantifying and ultrasonically treating to obtain a nano-cellulose solution;
(3) adding water and a dispersing agent into a glass fiber raw material, uniformly dispersing to obtain a slurry, and sequentially removing slag, diluting, forming and dehydrating to form a wet paper sheet with uniform thickness.
(4) And coating the nano-cellulose solution on the surface of the glass fiber paper in a coating mode to form a nano-cellulose coating.
(5) And (5) drying and forming.
The fibrillatable plant fiber pulp board in the step (1) is one or more of softwood pulp, hardwood pulp, cotton pulp, jute pulp, mercerized wood pulp, mercerized cotton pulp or mercerized jute pulp; the invention adopts the plant fiber as the raw material, thus saving the cost.
In the step (1), the soaking time of the pulp board is more than 4h, the concentration of the fiber suspension is 1-10%, the rotating speed of a fluffer is 1000-;
the physical method in the step (2) is one of a high-shearing force mechanical grinding method, a hot pressing method and a high-speed stirring method, and the chemical method is one of an acid hydrolysis method and an enzymolysis method;
the preferable preparation method of the nano-cellulose by using a TEMPO oxidation method is characterized in that the nano-cellulose is prepared by using the method, hydroxyl is oxidized into carboxyl, so that the nano-cellulose is negatively charged and has active functional groups, and when the nano-cellulose solution with the negatively charged and active functional groups is coated on a glass fiber substrate, the nano-cellulose solution and the glass fiber generate hydrogen bond action, so that the interlayer binding force between the nano-cellulose and the glass fiber is enhanced.
The diameter of the nano-cellulose prepared in the step (2) is 100-500 nm.
The concentration range of the nano-cellulose solution quantitatively obtained in the step (2) is 0.01-3%, and the more preferable concentration of the cellulose is 0.1-1.5%. The ultrasonic oscillation power is 200 + 10000KW, and the oscillation time is not less than 4h until a clarified and uniform solution is obtained;
the raw material of the glass fiber paper in the step (3) is preferably micro fiber cotton, and the diameter of the glass fiber is 0.8-1.5 mu m;
the dispersant in the step (3) is one or a mixture of more than two of a surfactant, a water-soluble high molecular compound or an acid.
The surfactant is quaternary ammonium salt or fatty acid salt and the like;
the acid is sulfuric acid, acetic acid, oxalic acid, etc.;
the water-soluble high molecular compound is polyoxyethylene, polyacrylamide and the like;
in the step (3), the concentration of the slurry is 0.5-5%, and the concentration after dilution is preferably 0.1-1%; the pH value of the slurry is 2-5;
the thickness of the glass fiber paper web obtained in the step (3) is preferably 0.1-0.5mm, and the thickness of the paper web is more preferably 0.25-0.35 mm;
the coating mode in the step (4) is one of roll coating and knife coating; the coating process simplifies the process, is simple to operate and is beneficial to industrial production.
And (5) drying in one or more of roller drying, infrared drying and hot air drying.
The nano-cellulose/glass fiber composite filter material prepared by the method can be used in the filtration fields of gas filtration, liquid filtration and the like.
In the following examples:
the liquid filtering efficiency is as per EN 13443-2-2007 mechanical filter for water conditioning equipment in buildings, part 2: particle ratings from 1 μm to 80 μm (80 μm excluded).
The air filtration efficiency is determined according to the regulations of GB/T19083-.
Example 1
(1) Soaking the needle-leaved wood commodity pulp board in deionized water for 4 hours to obtain pulp with the pulp concentration of 1 percent; and then putting the soaked pulp into a fluffer for fluffing for 20min, wherein the rotating speed of the fluffer is 1000 revolutions per minute, wringing out the pulp after fluffing, and balancing the moisture for 24h at the temperature of 4 ℃ for standby.
(2) The method comprises the steps of preparing nano-cellulose by a chemical TEMPO oxidation method, washing, and oscillating under 200KW power by ultrasonic waves to obtain a clear transparent solution with the concentration of the nano-cellulose of 0.1 wt%.
(3) Mixing microfiber glass wool and short glass fiber shreds according to a set proportion, adding water and sulfuric acid, and uniformly stirring by a high-frequency fluffer to obtain slurry with the concentration of 1.5 wt% and the pH value of 3.2; the obtained pulp is diluted into paper pulp suspension with the concentration of 0.45 wt% after deslagging, a wet paper sheet is formed after forming and dewatering by a fourdrinier, and a filter paper substrate is formed after drying, so that the thickness of the obtained glass fiber paper web is 0.25 mm;
(4) and (3) uniformly coating the nano cellulose solution obtained in the step (2) on the glass fiber filter paper substrate obtained in the step (3) through a roller coater.
(5) Drying by a drying cylinder to obtain the novel nano-cellulose/glass fiber composite filter material.
The nano-cellulose/glass fiber composite filter material obtained in example 1 has 85L/minPAO aerosol efficiency of 95.9941%, resistance of 89Pa and liquid 5um filtration accuracy of 99.97% measured by TSI 8130.
Example 2
(1) Soaking a hardwood commodity pulp board in deionized water for 6 hours to obtain pulp with the pulp concentration of 5%; and then putting the soaked pulp into a fluffer for fluffing for 30min, wherein the rotating speed of the fluffer is 2000r/min, wringing out the pulp after fluffing, and balancing the moisture for 24h at the temperature of 4 ℃ for standby.
(2) The nano-cellulose is prepared by a chemical method acid hydrolysis method, then washed and vibrated under 1000KW power by ultrasonic to obtain clear and transparent solution with the nano-cellulose concentration of 1.5 percent by weight.
(3) Mixing microfiber glass wool and short glass fiber shreds according to a set proportion, adding water and sulfuric acid, and uniformly stirring by a high-frequency fluffer to obtain slurry with the concentration of 1.0 wt% and the pH value of 3.0; the obtained pulp is diluted into paper pulp suspension with the concentration of 0.35 wt% after deslagging, a wet paper sheet is formed after forming and dewatering by a fourdrinier, and a filter paper substrate is formed after drying, so that the thickness of the obtained glass fiber paper web is 0.33 mm;
(4) and (3) uniformly coating the nano cellulose solution obtained in the step (2) on the glass fiber filter paper substrate obtained in the step (3) through a roller coater.
(5) And infrared drying to obtain the novel nano-cellulose/glass fiber composite filter material.
The nano-cellulose/glass fiber composite filter material obtained in the embodiment has 85L/minPAO aerosol efficiency of 90.1241%, resistance of 59Pa and liquid 5um filtration precision of 95.77% measured by TSI 8130.
Example 3
(1) Soaking a cotton pulp commodity pulp board in deionized water for 4 hours to obtain pulp with the pulp concentration of 10 percent; and then putting the soaked pulp into a fluffer for fluffing for 60min, wherein the rotating speed of the fluffer is 1500 rpm, wringing the pulp after fluffing, and balancing the moisture for 32h at the temperature of 20 ℃ for standby.
(2) The method comprises the steps of preparing nano-cellulose by a physical method high-shear mechanical grinding method, washing, and oscillating under 150KW power by ultrasonic waves to obtain a clear transparent solution with the nano-cellulose concentration of 1 wt%.
(3) Mixing microfiber glass wool and short glass fiber shreds according to a set proportion, adding water and sulfuric acid, and uniformly stirring by a high-frequency fluffer to obtain slurry with the concentration of 3.5 wt% and the pH value of 4; the obtained pulp is diluted into paper pulp suspension with the concentration of 0.5 wt% after deslagging, a wet paper sheet is formed after forming and dehydration by a fourdrinier, and a filter paper base material is formed after drying, so that the thickness of the obtained glass fiber paper web is 0.4 mm;
(4) and (3) uniformly coating the nano cellulose solution obtained in the step (2) on the glass fiber filter paper substrate obtained in the step (3) through a knife coater.
(5) Drying by a drying cylinder to obtain the novel nano-cellulose/glass fiber composite filter material.
The nano-cellulose/glass fiber composite filter material obtained in the embodiment has 85L/minPAO aerosol efficiency 95.5519%, resistance 112Pa and liquid 5um filtration precision 98.11% measured by TSI 8130.
Example 4
(1) Soaking the needle-leaved wood commodity pulp board in deionized water for 8 hours to obtain pulp with the pulp concentration of 1 percent; and then putting the soaked pulp into a fluffer for fluffing for 20min, wherein the rotating speed of the fluffer is 1000 revolutions per minute, wringing out the pulp after fluffing, and balancing the moisture at 25 ℃ for 48h for later use.
(2) The method comprises the steps of preparing nano-cellulose by a chemical TEMPO oxidation method, washing, and oscillating under the power of 10000KW ultrasonic waves to obtain a clear transparent solution with the concentration of the nano-cellulose of 1.5 percent by weight.
(3) Mixing microfiber glass wool and short glass fiber shreds according to a set proportion, adding water and sulfuric acid, and uniformly stirring by a high-frequency fluffer to obtain slurry with the concentration of 1.8 wt% and the pH value of 2.8; the obtained pulp is diluted into paper pulp suspension with the concentration of 0.38 wt% after deslagging, a wet paper sheet is formed after forming and dewatering by a fourdrinier, and a filter paper substrate is formed after drying, so that the thickness of the obtained glass fiber paper web is 0.3 mm;
(4) and (3) uniformly coating the nano cellulose solution obtained in the step (2) on the glass fiber filter paper substrate obtained in the step (3) through a knife coater.
(5) Drying by a drying cylinder to obtain the novel nano-cellulose/glass fiber composite filter material.
The nano-cellulose/glass fiber composite filter material obtained in the embodiment has 85L/minPAO aerosol efficiency of 98.9941%, resistance of 102Pa and liquid 5um filtration precision of 99.53% measured by TSI 8130.
From examples 1 to 4, it can be seen that the nano-cellulose glass fiber composite filter material prepared by the method of the present invention has the properties of low resistance, high filtration precision, etc., and the preparation method of the present invention avoids the use of organic reagents, simplifies the process, and is beneficial to industrial production.
The embodiments of the present invention are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention. That is, all equivalent changes and modifications made according to the content of the claims of the present invention should be regarded as the technical scope of the present invention.
Claims (10)
1. A method for preparing a nano-cellulose glass fiber composite filter material is characterized by comprising the following steps:
step (1): preparing a nano cellulose solution;
step (2): preparing a wet glass fiber paper sheet;
and (3): coating the nano cellulose solution obtained in the step (1) on the surface of the glass fiber wet paper sheet obtained in the step (2) in a coating mode;
and (4): drying and forming to obtain the nano cellulose glass fiber composite filter material.
2. The method according to claim 1, characterized in that said step (1) comprises in particular:
step (1-1): soaking a plant fiber pulp board capable of fibrillating in water, defibering by a defibering machine, dispersing in the water to obtain uniform fiber suspension, filtering, wringing, and balancing moisture for later use;
step (1-2): processing by physical or chemical method to obtain nano-cellulose, washing, quantifying, and ultrasonically treating to obtain nano-cellulose solution.
3. The method as claimed in claim 2, wherein the fibrillatable plant fiber pulp sheet in the step (1-1) is one or more of softwood pulp, hardwood pulp, cotton pulp, hemp pulp, mercerized wood pulp, mercerized cotton pulp or mercerized hemp pulp;
the soaking time of the pulp board in the step (1-1) is more than 4h, the rotating speed of the fluffer is 1000-2000r/min, the fluffing time is 10-60min, the concentration of the obtained fiber suspension is 1-10%, the equilibrium moisture time is more than 24h, and the equilibrium moisture temperature is 4-25 ℃.
4. The method according to claim 2, characterized in that the chemical process is a TEMPO oxidation process.
5. The method according to claim 2, wherein the concentration of the nano-cellulose solution quantitatively obtained in the step (1-2) is in the range of 0.01-3%, preferably 0.1-1.5%;
the ultrasonic oscillation power of the ultrasonic is 200-10000KW, and the oscillation time is not less than 4h until a clarified and uniform solution is obtained.
6. The method according to claim 1, wherein the step (2) of preparing the glass fiber wet paper is specifically:
adding water and a dispersing agent into a glass fiber raw material, uniformly dispersing to obtain slurry, and sequentially removing slag, diluting, forming and dehydrating to form wet paper sheets.
7. The method according to claim 6, characterized in that the glass fiber paper stock is preferably micro fiber cotton;
the dispersant is one or a mixture of more than two of a surfactant, a water-soluble high molecular compound or an acid;
preferably, the surfactant is quaternary ammonium salt or fatty acid salt, the acid is sulfuric acid, acetic acid or oxalic acid, and the water-soluble high molecular compound is polyoxyethylene or polyacrylamide;
in the step (2), the concentration of the slurry is 0.5-5%, the concentration after dilution is 0.1-1%, and the pH of the slurry is 2-5;
the thickness of the glass fiber paper web obtained in the step (2) is 0.1-0.5mm, and the preferred thickness of the paper web is 0.25-0.35 mm.
8. The method according to claim 1, wherein the coating manner in the step (3) is one of roll coating and knife coating;
and (4) drying in one or more of roller drying, infrared drying and hot air drying.
9. A nanocellulose glass fibre composite filter material prepared by the method of any one of claims 1 to 8, comprising a glass fibre substrate and a nanocellulose layer coated on the surface of the glass fibre substrate.
10. Use of a nanocellulose glass fibre composite filter material prepared by the method of any one of claims 1 to 8 for filtration, preferably gas or liquid filtration.
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