CN112048939B - Filter paper for menthol production and preparation method thereof - Google Patents
Filter paper for menthol production and preparation method thereof Download PDFInfo
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- CN112048939B CN112048939B CN202010807389.6A CN202010807389A CN112048939B CN 112048939 B CN112048939 B CN 112048939B CN 202010807389 A CN202010807389 A CN 202010807389A CN 112048939 B CN112048939 B CN 112048939B
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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
- D21H27/00—Special paper not otherwise provided for, e.g. made by multi-step processes
- D21H27/08—Filter paper
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21D—TREATMENT OF THE MATERIALS BEFORE PASSING TO THE PAPER-MAKING MACHINE
- D21D1/00—Methods of beating or refining; Beaters of the Hollander type
- D21D1/02—Methods of beating; Beaters of the Hollander type
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- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21F—PAPER-MAKING MACHINES; METHODS OF PRODUCING PAPER THEREON
- D21F11/00—Processes for making continuous lengths of paper, or of cardboard, or of wet web for fibre board production, on paper-making machines
- D21F11/14—Making cellulose wadding, filter or blotting paper
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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
-
- 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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/03—Non-macromolecular organic compounds
- D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
- D21H17/06—Alcohols; Phenols; Ethers; Aldehydes; Ketones; Acetals; Ketals
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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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/34—Synthetic macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/37—Polymers of unsaturated acids or derivatives thereof, e.g. polyacrylates
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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
- D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
- D21H17/20—Macromolecular organic compounds
- D21H17/33—Synthetic macromolecular compounds
- D21H17/46—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D21H17/47—Condensation polymers of aldehydes or ketones
- D21H17/49—Condensation polymers of aldehydes or ketones with compounds containing hydrogen bound to nitrogen
- D21H17/51—Triazines, e.g. melamine
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Abstract
The invention discloses filter paper for menthol production and a preparation method thereof, which relate to the technical field of filter paper preparation and sequentially comprise a coarse filter layer and a fine filter layer from top to bottom; the coarse filter layer comprises the following components in parts by mass: 80-90 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 10-20 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m and 3-5 parts of water-shrinkable polyacrylate particles; 2-4 parts of a binder; the fine filtering layer comprises the following components in parts by mass: 20-30 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 70-80 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m, 4-6 parts of aerogel particles, 0.5-1 part of ethylene glycol diglycidyl ether and 3-5 parts of binder; the filter paper prepared by the method can effectively remove impurities in the filter paper by water backwashing, has high repeated utilization rate, is suitable for menthol production, and reduces the cost.
Description
Technical Field
The invention relates to the technical field of filter paper preparation, in particular to filter paper for menthol production and a preparation method thereof.
Background
The mint is a mint plant of the family Labiatae, is a traditional Chinese medicine with wide application and is also one of three major spices in the world. The menthol is extracted from stems and leaves of traditional Chinese medicine mint, has special cool fragrance, is pungent in flavor, and is an aromatic drug, a seasoning drug and a wind-expelling drug after cooling. Can be used for relieving discomfort and pain due to skin or mucosa cold feeling, has effects of dispersing stagnated liver qi, and promoting bile flow, and can be used for treating headache and inflammation of nose, pharynx, and larynx by oral administration. In the preparation process of the menthol, in order to ensure the extraction rate and the prepared menthol has high purity, the menthol needs to be subjected to repeated freezeout, dehydration, filtration and crystallization during the production of the menthol, and repeated impurity removal is performed.
For example, a qualitative filter paper and a manufacturing process thereof disclosed in chinese patent document, whose publication No. CN103911911A discloses a qualitative filter paper and a manufacturing process thereof, comprising the following materials in parts by mass: 30-50 parts of sulfate bleached softwood pulp, 20-40 parts of sulfate bleached hardwood pulp, 1-3 parts of wet strength agent and 0.2-0.4 part of whitening agent. The long fibers and the short fibers are mixed for use, so that the defects caused by the fact that the filter paper is made of a single fiber are overcome. But the reproducibility in the filter paper is poor and the filter paper is easily broken in the presence of pressure filtration and mechanical impurities.
Disclosure of Invention
The invention provides a filter paper for menthol production and a preparation method thereof, aiming at solving the problems that the filter paper cannot be used repeatedly for many times during the existing menthol preparation and filtration, if the filter paper is not replaced for a long time, the mechanical impurities can not only reduce the filtration efficiency, but also increase the impurities in the prepared menthol, and if the filter paper is replaced frequently, the production waste is easily caused due to more filtration times in the production process.
In order to achieve the purpose, the invention adopts the following technical scheme:
the filter paper for producing the menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence;
the coarse filter layer comprises the following components in parts by mass: 80-90 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 10-20 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m and 3-5 parts of water-shrinkable polyacrylate particles; 2-4 parts of a binder; the fine filtering layer comprises the following components in parts by mass: 20-30 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 70-80 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m, 4-6 parts of aerogel particles, 0.5-1 part of ethylene glycol diglycidyl ether and 3-5 parts of binder.
According to the invention, the filter paper for producing the menthol is divided into an upper layer and a lower layer, wherein the upper layer is a coarse filter layer, has loose pore size and is used for intercepting large-particle or flaky mechanical impurities; the lower layer is a fine filtering layer for intercepting fine particles.
In the upper coarse filter layer, the invention adopts a mode of mixing and matching large-diameter alkali-free glass fiber cotton and small-diameter alkali-free glass fiber cotton, and the proportion of the large-diameter alkali-free glass fiber cotton is larger than that of the small-diameter alkali-free glass fiber cotton, so that after pulping and forming, the prepared glass fiber layer has a loose pore diameter, a large pore diameter and a high pore diameter rate, and can filter large-particle or flake mechanical impurities; in the upper coarse filter layer of the filter paper, the pores contain water-shrinkable polyacrylate particles, so that the water-shrinkable polyacrylate particles shrink when encountering water in the process of back washing with water, the pore diameter of the upper coarse filter layer is enlarged, mechanical impurities embedded in the fiber layer can be washed out, the water-shrinkable polyacrylate particles can restore to the original size after drying, and the pore diameter of the upper coarse filter layer also restores to the normal filtering level.
In the lower fine filtering layer, the invention also adopts a mode of mixing and matching the large-diameter alkali-free glass fiber cotton and the small-diameter alkali-free glass fiber cotton, in the proportion, the content of the small-diameter alkali-free glass fiber cotton is greater than that of the large-diameter alkali-free glass fiber cotton, after pulping and forming, the large-diameter alkali-free glass fiber cotton plays a role of a three-dimensional framework structure, and the small-diameter alkali-free glass fiber cotton is randomly distributed and wound on the three-dimensional framework structure to refill and divide the aperture, so that the lower fine filtering layer with smaller aperture is obtained, and meanwhile, the porosity is maintained at a higher level. Meanwhile, in order to further increase the fine filtering effect of the lower fine filtering layer, aerogel particles are added into the lower fine filtering layer, have developed pore structures and are filled in the fiber layer, so that the filtering precision of the lower fine filtering layer can be greatly improved, and the mechanical strength of the lower fine filtering layer can also be improved.
Therefore, when the filter paper is used for filtering, the menthol naphtha firstly passes through the upper coarse filter layer, large-particle mechanical impurities are intercepted, and then the naphtha flows out of the lower fine filter layer to intercept some small impurities with lower content.
Preferably, the thickness of the coarse filter layer is 0.13-0.18mm, and the thickness of the fine filter layer is 0.22-0.28mm.
Preferably, the binder is an acrylic resin.
A preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing the alkali-free glass fiber cotton with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.5-3%, the pH value is 3-3.5, and the pulp is pulped until the beating degree is 40-45 DEG SR;
b: and (3) wet forming: deslagging the slurry, diluting the slurry until the mass concentration is 0.2-0.3%, adding water to obtain condensed acrylate particles, and then carrying out wet forming to obtain wet paper;
c: sizing: adding acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filtering layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: dispersing alkali-free glass fiber cotton into a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 1.5-2wt% to obtain slurry, wherein the mass concentration of the slurry is 10-12%, stirring for 5-8h at the temperature of 40-60 ℃, filtering, washing and drying to prepare amino modified glass fiber cotton;
b: dispersing and pulping: mixing, pulping and dispersing amino modified glass fiber cotton, water and sulfuric acid, wherein the mass concentration of the pulp is 2.5-3%, the pH value is 3-3.5, and pulping until the beating degree is 50-55 DEG SR;
c: and (3) wet forming: deslagging the slurry, diluting the slurry to a mass concentration of 0.2-0.3%, adding aerogel particles and ethylene glycol diglycidyl ether, and then carrying out wet forming to obtain wet paper;
d: sizing: adding acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and smart filter layer:
and (3) attaching the blank paper of the coarse filtering layer and the blank paper of the fine filtering layer, and then performing vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol.
In the preparation process, the blank paper of the coarse filter layer and the blank paper of the fine filter layer are respectively prepared, and then the blank paper of the coarse filter layer and the blank paper of the fine filter layer are attached to be subjected to vacuum suction dehydration, drying and drying to prepare the filter paper. In the preparation process of the fine filtering layer blank paper, the alkali-free glass fiber cotton is firstly subjected to silane modification, then the ethylene glycol diglycidyl ether is added while the aerogel particles are added, and at the moment, the active groups at two ends of the ethylene glycol diglycidyl ether can firmly connect the aerogel particles and the glass fibers together to play a good bridging role and prevent the shedding of the aerogel particles in the forming and dewatering processes.
Preferably, the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate, adding catalyst, mixing thoroughly, placing in a mold, curing at 90-100 deg.C for 2-5h, taking out, stretching at 110-120 deg.C until the deformation is 200-250%, cooling to 0-5 deg.C, keeping the temperature, and processing into granule.
According to the invention, the water-shrinkable polyacrylate particles are prepared by curing the polyethylene glycol diacrylate and the cyclohexyl methacrylate, wherein the polyethylene glycol diacrylate belongs to hydrophilic crystalline substances, so that the prepared polyacrylate material takes the cyclohexyl methacrylate with high glass transition temperature as a skeleton material and the polyethylene glycol diacrylate as a driving phase, when the material encounters water, a polyethylene glycol diacrylate chain segment is gradually dissolved, a molecular chain is curled, the material is shrunk, and when the material slowly returns to a dry state, the dissolved polyethylene glycol diacrylate chain segment is subjected to orientation crystallization due to internal force, and the material returns to the original state. Therefore, the water-shrinkable polyacrylate particles prepared by the method have the effect of responding to water, and can reversibly change the shape during dry and wet cycles.
Preferably, the mass ratio of the polyethylene glycol diacrylate to the cyclohexyl methacrylate is 2-2.5.
Preferably, the catalyst is benzoyl peroxide, and the addition amount is 1-3wt% of the total amount.
Preferably, the aerogel particles are prepared by the following method: placing the nano cellulose fibers in deionized water, adding hexamethoxy melamine formaldehyde resin and phosphoric acid after stirring to adjust the pH value to 4-4.5, then adding sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in a gamma-aminopropyl triethoxysilane aqueous solution, reacting for 10-20h at 20-30 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
According to the invention, when the aerogel particles are prepared, the hexamethoxy melamine formaldehyde resin is added in the preparation process, and the hexamethoxy melamine formaldehyde resin can be chemically crosslinked with hydroxyl on the surface of the fiber, so that the mechanical property of the aerogel can be improved, and the structural integrity of the aerogel can be enhanced. Meanwhile, sodium bicarbonate is added in the preparation process, and is gradually decomposed in the stirring process, so that the prepared aerogel particles have higher porosity, and the surfaces of the aerogel particles are provided with active groups reacted with ethylene glycol diglycidyl ether by performing amino modification on the aerogel particles by adopting gamma-aminopropyltriethoxysilane, so that the aerogel particles are more firmly connected to the surface of the glass fiber.
Preferably, the raw materials in parts by weight are as follows: 2-5 parts of nano cellulose fiber, 100-110 parts of deionized water, 0.5-1 part of hexamethoxy melamine formaldehyde resin and 0.1-0.3 part of sodium bicarbonate.
Preferably, the concentration of the gamma-aminopropyltriethoxysilane aqueous solution is 1.5-2wt%.
Therefore, the invention has the following beneficial effects: after the filter paper prepared by the method is used, impurities in the filter paper can be effectively removed by backwashing with water, the filter paper can be reused after being dried, the reuse rate is high, the method is suitable for menthol production, and the cost is reduced.
Detailed Description
The invention is further described with reference to specific embodiments.
General example:
a filter paper for producing menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.13-0.18mm, and the thickness of the fine filter layer is 0.22-0.28mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 80-90 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 10-20 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m, water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.5-3%, the pH value is 3-3.5, and the pulp is pulped until the beating degree is 40-45 DEG SR;
b: and (3) wet forming: removing slag of the slurry, diluting the slurry to the mass concentration of 0.2-0.3%, adding 3-5 parts of water-shrinkable polyacrylate particles, and then carrying out wet forming to obtain wet paper;
c: sizing: adding 2-4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filter layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing and dispersing 20-30 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm and 70-80 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m in a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 1.5-2wt% to obtain slurry, wherein the mass concentration of the slurry is 10-12%, stirring for 5-8h at the temperature of 40-60 ℃, filtering, washing and drying to prepare amino modified glass fiber cotton;
b: dispersing and pulping: mixing the amino modified glass fiber cotton with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.5-3%, the pH value is 3-3.5, and the pulp is pulped until the beating degree is 50-55 DEG SR;
c: and (3) wet forming: removing slag from the slurry, diluting the slurry to a mass concentration of 0.2-0.3%, adding 4-6 parts of aerogel particles and 0.5-1 part of ethylene glycol diglycidyl ether, and performing wet forming to obtain wet paper;
d: sizing: adding 3-5 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and smart filter layer:
attaching the rough filtering layer blank paper and the fine filtering layer blank, and then performing vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2-2.5, adding 1-3wt% of benzoyl peroxide as a catalyst, fully mixing, placing in a mold, curing at 90-100 ℃ for 2-5h, taking out, stretching at 110-120 ℃ until the deformation is 200-250%, cooling to 0-5 ℃, preserving heat and processing into granules;
the preparation method of the aerogel particles comprises the following steps: placing 2-5 parts of nano cellulose fiber in 100-110 parts of deionized water, stirring, adding 0.5-1 part of hexamethoxy melamine formaldehyde resin and phosphoric acid to adjust the pH value to 4-4.5, then adding 0.1-0.3 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in 1.5-2wt% of gamma-aminopropyl triethoxysilane aqueous solution, reacting at 20-30 ℃ for 10-20h, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
Example 1: a filter paper for producing menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.18mm, and the thickness of the fine filter layer is 0.22mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 85 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 15 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.2, and the pulp is pulped until the beating degree is 43 DEG SR; b: and (3) wet forming: removing slag of the slurry, diluting the slurry until the mass concentration is 0.25%, adding 4 parts of water-shrinkable polyacrylate particles, and performing wet forming to obtain wet paper;
c: sizing: adding 3 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filtering layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing 25 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 75 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m, dispersing the mixture in a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 2wt% to obtain slurry, wherein the mass concentration of the slurry is 11%, stirring the slurry at 50 ℃ for 7 hours, and then filtering, washing and drying the mixture to prepare the amino modified glass fiber cotton;
b: dispersing and pulping: mixing, pulping and dispersing amino modified glass fiber cotton, water and sulfuric acid, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.3, and pulping until the beating degree is 53-degree SR;
c: and (3) wet forming: removing slag from the slurry, diluting the slurry to a mass concentration of 0.25%, adding 5 parts of aerogel particles and 0.8 part of ethylene glycol diglycidyl ether, and performing wet forming to obtain wet paper;
d: sizing: adding 4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and fine filtration layer:
attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2.3, adding 2wt% of benzoyl peroxide as a catalyst, fully mixing, placing in a mold, curing at 96 ℃ for 3h, taking out, stretching at 115 ℃ until the deformation reaches 230%, cooling to 0 ℃, preserving heat, and processing into granules;
the preparation method of the aerogel particles comprises the following steps: placing 3 parts of nano cellulose fiber in 105 parts of deionized water, adding 0.7 part of hexamethoxy melamine formaldehyde resin and phosphoric acid after stirring to adjust the pH value to 4.3, then adding 0.2 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in 1.8wt% of gamma-aminopropyl triethoxysilane aqueous solution, reacting for 15 hours at 25 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
Example 2: a filter paper for producing menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.15mm, and the thickness of the fine filter layer is 0.26mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 80 parts of alkali-free glass fiber cotton with the diameter of 4.5mm and 20 parts of alkali-free glass fiber cotton with the diameter of 0.4 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.5%, the pH value is 3, and pulping is carried out until the beating degree is 40 DEG SR;
b: and (3) wet forming: removing slag of the slurry, diluting the slurry until the mass concentration is 0.2%, adding 3 parts of water-shrinkable polyacrylate particles, and performing wet forming to obtain wet paper;
c: sizing: adding 2 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filter layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing and dispersing 20 parts of alkali-free glass fiber cotton with the diameter of 4.5mm and 80 parts of alkali-free glass fiber cotton with the diameter of 0.3 mu m into gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 1.5wt% to obtain slurry, wherein the mass concentration of the slurry is 10%, stirring for 8 hours at 40 ℃, filtering, washing and drying to prepare the amino modified glass fiber cotton;
b: dispersing and pulping: mixing, pulping and dispersing amino modified glass fiber cotton, water and sulfuric acid, wherein the mass concentration of the pulp is 2.5%, the pH value is 3, and pulping until the beating degree is 50 DEG SR;
c: and (3) wet forming: removing residues from the slurry, diluting the slurry to a mass concentration of 0.2%, adding 4 parts of aerogel particles and 0.5 part of ethylene glycol diglycidyl ether, and performing wet forming to obtain wet paper;
d: sizing: adding 3 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and smart filter layer:
attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2;
the preparation method of the aerogel particles comprises the following steps: placing 2 parts of nanocellulose fibers in 100 parts of deionized water, adding 0.5 part of hexamethoxymelamine formaldehyde resin and phosphoric acid after stirring to adjust the pH to 4.5, then adding 0.1 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in 1.5wt% of gamma-aminopropyltriethoxysilane aqueous solution, reacting for 20 hours at 20 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
Example 3: a filter paper for producing menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.16mm, and the thickness of the fine filter layer is 0.23mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 90 parts of alkali-free glass fiber cotton with the diameter of 5.0mm and 10 parts of alkali-free glass fiber cotton with the diameter of 0.4 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 3%, the pH value is 3.5, and the pulp is pulped until the beating degree is 45 DEG SR;
b: and (3) wet forming: removing slag of the slurry, diluting the slurry until the mass concentration is 0.3%, adding 5 parts of water-shrinkable polyacrylate particles, and performing wet forming to obtain wet paper;
c: sizing: adding 4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filter layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing and dispersing 30 parts of alkali-free glass fiber cotton with the diameter of 5.0mm and 70 parts of alkali-free glass fiber cotton with the diameter of 0.4 mu m into gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 2wt% to obtain slurry, wherein the mass concentration of the slurry is 12%, stirring for 8 hours at 60 ℃, filtering, washing and drying to prepare the amino modified glass fiber cotton;
b: dispersing and pulping: mixing, pulping and dispersing amino modified glass fiber cotton, water and sulfuric acid, wherein the mass concentration of the pulp is 3%, the pH value is 3.5, and pulping until the beating degree is 55-degree SR;
c: and (3) wet forming: removing residues from the slurry, diluting the slurry to a mass concentration of 0.3%, adding 6 parts of aerogel particles and 1 part of ethylene glycol diglycidyl ether, and performing wet forming to obtain wet paper;
d: sizing: adding 5 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and smart filter layer:
attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2.5; the preparation method of the aerogel particles comprises the following steps: placing 5 parts of nano cellulose fiber in 110 parts of deionized water, adding 1 part of hexamethoxy melamine formaldehyde resin and phosphoric acid after stirring to adjust the pH to 4.5, then adding 0.3 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in 2wt% of gamma-aminopropyl triethoxysilane aqueous solution, reacting for 10 hours at 30 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
Example 4: a filter paper for producing menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.13mm, and the thickness of the fine filter layer is 0.28mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 86 parts of alkali-free glass fiber cotton with the diameter of 4.8mm and 13 parts of alkali-free glass fiber cotton with the diameter of 0.32 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.2, and pulping is carried out until the beating degree is 44 DEG SR;
b: and (3) wet forming: removing slag of the slurry, diluting the slurry until the mass concentration is 0.7%, adding 4 parts of water-shrinkable polyacrylate particles, and performing wet forming to obtain wet paper;
c: sizing: adding 3 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filter layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing and dispersing 28 parts of alkali-free glass fiber cotton with the diameter of 4.8mm and 77 parts of alkali-free glass fiber cotton with the diameter of 0.31 mu m in a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 1.7wt% to obtain slurry, wherein the mass concentration of the slurry is 11%, stirring for 7 hours at 48 ℃, filtering, washing and drying to prepare amino modified glass fiber cotton;
b: dispersing and pulping: mixing the amino modified glass fiber cotton with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.7%, the pH value is 3.3, and pulping is carried out until the beating degree is 52 DEG SR;
c: and (3) wet forming: removing slag from the slurry, diluting the slurry to a mass concentration of 0.27%, adding 5 parts of aerogel particles and 0.8 part of ethylene glycol diglycidyl ether, and performing wet forming to obtain wet paper;
d: sizing: adding 4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and fine filtration layer:
attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2.1, adding 1.7wt% of benzoyl peroxide as a catalyst, fully mixing, placing in a mold, curing at 97 ℃ for 4 hours, taking out, stretching at 118 ℃ until the deformation reaches 230%, cooling to 0 ℃, preserving heat, and processing into granules; the preparation method of the aerogel particles comprises the following steps: putting 4 parts of nano cellulose fiber into 117 parts of deionized water, adding 0.7 part of hexamethoxymelamine formaldehyde resin and phosphoric acid after stirring to adjust the pH to 4.2, then adding 0.2 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles into 1.8wt% of gamma-aminopropyltriethoxysilane aqueous solution, reacting for 14 hours at 27 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
Comparative example 1: a filter paper for menthol production comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.18mm, and the thickness of the fine filter layer is 0.22mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filtering layer:
a: dispersing and pulping: mixing 85 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 15 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.2, and the pulp is pulped until the beating degree is 43 DEG SR;
b: and (3) wet forming: deslagging the slurry, diluting the slurry until the mass concentration is 0.25%, and then carrying out wet forming to obtain wet paper;
c: sizing: adding 3 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filter layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing 25 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 75 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m, dispersing the mixture in a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 2wt% to obtain slurry, wherein the mass concentration of the slurry is 11%, stirring the slurry at 50 ℃ for 7 hours, and then filtering, washing and drying the mixture to prepare the amino modified glass fiber cotton;
b: dispersing and pulping: mixing the amino modified glass fiber cotton with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.3, and pulping is carried out until the beating degree is 53 DEG SR;
c: and (3) wet forming: removing slag from the slurry, diluting the slurry to a mass concentration of 0.25%, adding 5 parts of aerogel particles and 0.8 part of ethylene glycol diglycidyl ether, and performing wet forming to obtain wet paper;
d: sizing: adding 4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and smart filter layer:
attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the aerogel particles comprises the following steps: placing 3 parts of nano cellulose fiber in 105 parts of deionized water, adding 0.7 part of hexamethoxy melamine formaldehyde resin and phosphoric acid after stirring to adjust the pH value to 4.3, then adding 0.2 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in 1.8wt% of gamma-aminopropyl triethoxysilane aqueous solution, reacting for 15 hours at 25 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles.
Comparative example 2: a filter paper for menthol production comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.18mm, and the thickness of the fine filter layer is 0.22mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 85 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 15 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.2, and the pulp is pulped until the beating degree is 43 DEG SR;
b: and (3) wet forming: removing slag from the slurry, diluting the slurry until the mass concentration is 0.25%, adding 4 parts of water-shrinkable polyacrylate particles, and performing wet forming to obtain wet paper;
c: sizing: adding 3 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filter layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: mixing 25 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 75 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m, dispersing the mixture in a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 2wt% to obtain slurry, wherein the mass concentration of the slurry is 11%, stirring the slurry at 50 ℃ for 7 hours, and then filtering, washing and drying the mixture to prepare the amino modified glass fiber cotton;
b: dispersing and pulping: mixing, pulping and dispersing amino modified glass fiber cotton, water and sulfuric acid, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.3, and pulping until the beating degree is 53-degree SR;
c: and (3) wet forming: deslagging the slurry, diluting the slurry until the mass concentration is 0.25%, and then carrying out wet forming to obtain wet paper;
d: sizing: adding 4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and fine filtration layer:
attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2.3, adding 2wt% of benzoyl peroxide as a catalyst, fully mixing, placing in a mold, curing at 96 ℃ for 3h, taking out, stretching at 115 ℃ until the deformation reaches 230%, cooling to 0 ℃, preserving heat, and processing into granules.
Comparative example 3: a filter paper for producing menthol comprises a coarse filter layer and a fine filter layer from top to bottom in sequence; the thickness of the coarse filter layer is 0.18mm, and the thickness of the fine filter layer is 0.22mm;
a preparation method of filter paper for menthol production comprises the following preparation steps:
(1) Preparing a coarse filter layer:
a: dispersing and pulping: mixing 85 parts of alkali-free glass fiber cotton with the diameter of 4.7mm and 15 parts of alkali-free glass fiber cotton with the diameter of 0.35 mu m with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.2, and the pulp is pulped until the beating degree is 43 DEG SR;
b: and (3) wet forming: removing slag of the slurry, diluting the slurry until the mass concentration is 0.25%, adding 4 parts of water-shrinkable polyacrylate particles, and performing wet forming to obtain wet paper;
c: sizing: adding 3 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filtering layer;
(2) Preparing a fine filtering layer:
a: dispersing and pulping: mixing, pulping and dispersing amino modified glass fiber cotton, water and sulfuric acid, wherein the mass concentration of the pulp is 2.8%, the pH value is 3.3, and pulping until the beating degree is 53-degree SR;
b: and (3) wet forming: deslagging the slurry, diluting the slurry to a mass concentration of 0.25%, adding 5 parts of aerogel particles and 0.8 part of ethylene glycol diglycidyl ether, and then carrying out wet forming to obtain wet paper;
c: sizing: adding 4 parts of acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and smart filter layer:
attaching the rough filtering layer blank paper and the fine filtering layer blank, and then performing vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol crystal;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate according to a mass ratio of 2.3, adding 2wt% of benzoyl peroxide as a catalyst, fully mixing, placing in a mold, curing at 96 ℃ for 3h, taking out, stretching at 115 ℃ until the deformation reaches 230%, cooling to 0 ℃, preserving heat, and processing into granules;
the preparation method of the aerogel particles comprises the following steps: placing 3 parts of nano cellulose fiber in 105 parts of deionized water, stirring, adding 0.7 part of hexamethoxy melamine formaldehyde resin and phosphoric acid to adjust the pH to 4.3, then adding 0.2 part of sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, and preparing to obtain the aerogel particles.
The filter paper prepared in the above examples and comparative examples is subjected to a performance test, and the test standard CRAA431.3; wherein the post-use representation in the table is for menthol filtration and back-flushed with water and dried.
As can be seen from the above data, the filter paper prepared in the example has small change of the filtration resistance after use, and the filter paper prepared in the comparative example 1 is different from the filter paper prepared in the example 1 in that water is not added to shrink polyacrylate particles during the preparation of the coarse filter layer, so that the filtration resistance after use is obviously increased, which indicates that the mechanical impurities cannot be effectively washed away during the backflushing after use; comparative example 2 and comparative example 3 are different from example 1 in that aerogel particles are not added when preparing the fine filtration layer or are not modified when preparing the aerogel particles, so that the prepared filter paper easily falls off when preparing the filter paper due to no aerogel particles or the added aerogel particles due to non-modification, resulting in a decrease in overall filtration performance.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and all simple modifications, alterations and equivalents of the above embodiments according to the technical spirit of the present invention are still within the protection scope of the technical solution of the present invention.
Claims (4)
1. The filter paper for producing the menthol is characterized by comprising a coarse filter layer and a fine filter layer from top to bottom in sequence;
the coarse filter layer comprises the following components in parts by mass: 80-90 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 10-20 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m and 3-5 parts of water-shrinkable polyacrylate particles; 2-4 parts of a binder;
the fine filtering layer comprises the following components in parts by mass: 20-30 parts of alkali-free glass fiber cotton with the diameter of 4.5-5.0mm, 70-80 parts of alkali-free glass fiber cotton with the diameter of 0.3-0.4 mu m, 4-6 parts of aerogel particles, 0.5-1 part of ethylene glycol diglycidyl ether and 3-5 parts of binder;
the preparation method of the aerogel particles comprises the following steps: placing the nano cellulose fibers in deionized water, adding hexamethoxy melamine formaldehyde resin and phosphoric acid after stirring to adjust the pH value to 4-4.5, then adding sodium bicarbonate, fully stirring, freeze-drying, grinding into micron-sized particles, then immersing the micron-sized particles in a gamma-aminopropyl triethoxysilane aqueous solution, reacting for 10-20h at 20-30 ℃, washing after the reaction is finished, and freeze-drying to prepare the aerogel particles, wherein the raw materials in parts by weight are as follows: 2-5 parts of nano cellulose fiber, 100-110 parts of deionized water, 0.5-1 part of hexamethoxy melamine formaldehyde resin, 0.1-0.3 part of sodium bicarbonate, wherein the concentration of the gamma-aminopropyl triethoxysilane aqueous solution is 1.5-2wt%;
the preparation method of the water-shrinkable polyacrylate particles comprises the following steps: mixing polyethylene glycol diacrylate and cyclohexyl methacrylate, adding a catalyst, fully mixing, placing in a mold, curing at 90-100 ℃ for 2-5h, taking out, stretching at 110-120 ℃ until the deformation is 200-250%, then reducing to 0-5 ℃, preserving heat and processing into particles, wherein the mass ratio of the polyethylene glycol diacrylate to the cyclohexyl methacrylate is 2-2.5.
2. The filter paper for menthol production according to claim 1, wherein the thickness of the coarse filtration layer is 0.13-0.18mm, and the thickness of the fine filtration layer is 0.22-0.28mm.
3. The filter paper for menthol production according to claim 1, wherein the binder is acrylic resin.
4. A method for preparing filter paper for menthol production according to any one of claims 1 to 3, comprising the following steps:
(1) Preparing a coarse filtering layer:
a: dispersing and pulping: mixing alkali-free glass fiber cotton with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.5-3%, the pH value is 3-3.5, and pulping until the beating degree is 40-45 DEG SR;
b: and (3) wet forming: deslagging the slurry, diluting the slurry until the mass concentration is 0.2-0.3%, adding water to obtain condensed acrylate particles, and then carrying out wet forming to obtain wet paper;
c: sizing: adding acrylate emulsion into the wet paper for sizing to obtain blank paper of the coarse filtering layer;
(2) Preparing a fine filtering layer:
a: modifying glass fiber: dispersing alkali-free glass fiber cotton in a gamma-aminopropyltriethoxysilane aqueous solution with the concentration of 1.5-2wt% to obtain slurry, wherein the mass concentration of the slurry is 10-12%, stirring for 5-8h at the temperature of 40-60 ℃, filtering, washing and drying to prepare amino modified glass fiber cotton;
b: dispersing and pulping: mixing the amino modified glass fiber cotton prepared in the step (a) with water and sulfuric acid, pulping and dispersing, wherein the mass concentration of the pulp is 2.5-3%, the pH value is 3-3.5, and pulping until the beating degree is 50-55 DEG SR;
c: and (3) wet forming: deslagging the slurry, diluting the slurry to a mass concentration of 0.2-0.3%, adding aerogel particles and ethylene glycol diglycidyl ether, and then carrying out wet forming to obtain wet paper;
d: sizing: adding acrylate emulsion into the wet paper for sizing to obtain blank paper of the fine filtering layer;
(3) The laminating of coarse filtration layer and fine filtration layer:
and (3) attaching the blank paper of the coarse filtering layer and the blank of the fine filtering layer, and then carrying out vacuum suction dehydration, drying and drying to prepare the filter paper for producing the menthol.
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