CN109610238B - Flame-retardant cured filter paper and preparation method thereof - Google Patents
Flame-retardant cured filter paper and preparation method thereof Download PDFInfo
- Publication number
- CN109610238B CN109610238B CN201811376775.3A CN201811376775A CN109610238B CN 109610238 B CN109610238 B CN 109610238B CN 201811376775 A CN201811376775 A CN 201811376775A CN 109610238 B CN109610238 B CN 109610238B
- Authority
- CN
- China
- Prior art keywords
- flame
- filter paper
- parts
- pulp
- retardant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
- D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
- D21H11/02—Chemical or chemomechanical or chemothermomechanical pulp
- D21H11/04—Kraft or sulfate pulp
-
- 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
-
- 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
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
-
- 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
- D21H17/54—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen
- D21H17/56—Polyamines; Polyimines; Polyester-imides
-
- 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
- D21H17/63—Inorganic compounds
- D21H17/66—Salts, e.g. alums
-
- 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
-
- 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
- D21H19/24—Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
-
- 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
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/34—Ignifugeants
-
- 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
- D21H25/00—After-treatment of paper not provided for in groups D21H17/00 - D21H23/00
- D21H25/04—Physical treatment, e.g. heating, irradiating
- D21H25/06—Physical treatment, e.g. heating, irradiating of impregnated or coated paper
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Paper (AREA)
- Filtering Materials (AREA)
Abstract
The invention relates to the technical field of cured filter paper, and provides flame-retardant cured filter paper and a preparation method thereof, in order to improve the flame-retardant property of the filter paper and meet the application requirement of the filter paper on an engine, the flame-retardant cured filter paper is prepared by dipping a base paper body in a dipping solution, taking out the base paper body, and heating and curing the base paper body, wherein the base paper body is prepared from a composite wood pulp, polyetherimide powder, polyethyleneimine, melamine resin, a compatibilizer, a succinimide ashless dispersant and a defoaming agent, and the dipping solution is prepared from a thermosetting phenolic resin, a PCTA copolymer, a crosslinking agent, a flame retardant, a styrene-acrylic emulsion, methanol, isopropyl acetate and an organic silicon alcohol sodium salt. The flame-retardant cured filter paper disclosed by the invention is strong in flame retardant property, high-temperature resistant, strong in high-temperature dimensional stability, high in strength and filtering precision, simple in process, and easy to operate, and the prepared cured filter paper is suitable for being used as a filter element of an air filter of an engine, and the steps of the preparation method are saved.
Description
Technical Field
The invention relates to the technical field of cured filter paper, in particular to flame-retardant cured filter paper and a preparation method thereof.
Background
The air filter is positioned in an air inlet system of the engine, is arranged in front of an automobile carburetor or an air inlet pipe, plays a role in filtering dust and sand grains in air and ensures that sufficient and clean air enters the air cylinder. Common air filters include an inertial oil bath type air filter, a paper dry type air filter, a polyurethane filter element air filter, and the like. The filter element of the paper dry-type air filter is made of microporous filter paper treated by an adhesive, the adhesive forms a cured layer of the filter element, and the microporous filter paper is mainly made of plant fiber slurry. However, since the microporous filter paper has flammability, the filter element is easily burned when the engine cylinder is tempered, and the paper filter element is also burned when the engine sucks inflammable substances in the air, so that driving safety is affected, and the filter paper is required to have certain flame retardant property. In addition, due to the high temperature working environment of the engine, the filter paper is also required to have a certain high temperature resistance.
Chinese patent CN201521054157.9, the patent name "a flame retardant filter paper", discloses a flame retardant filter paper consisting of a primary filter layer, a secondary filter layer and a flame retardant layer permeating from the upper surface of the primary filter layer to the lower surface of the secondary filter layer, wherein a flame retardant layer is arranged between the primary filter layer and the secondary filter layer, and the flame retardant layer is made of halogen-free flame retardant, providing flame retardant property to the filter paper. However, the flame retardant effect is only from the flame retardant layer, and the flame resistance and temperature resistance of the primary filter layer and the secondary filter layer are general, so the overall flame retardant performance of the filter paper still needs to be improved.
Disclosure of Invention
In order to improve the flame retardant property of the filter paper and meet the application requirement of the filter paper on an engine, the invention aims to provide the flame-retardant cured filter paper which has stronger flame retardant property and stronger high temperature resistance and is suitable for being used as a filter element of an air filter of the engine.
The invention also aims to provide a preparation method of the flame-retardant cured filter paper.
The invention provides the following technical scheme:
the flame-retardant cured filter paper is prepared by taking out a base paper body after being soaked in a dipping solution and heating and curing, wherein:
the body of the base paper comprises the following components in parts by weight: 100-120 parts of composite wood pulp, 12-20 parts of polyetherimide powder, 3-5 parts of polyethyleneimine, 2-4 parts of melamine resin, 2-5 parts of compatibilizer, 4-6 parts of succinimide ashless dispersant and 2-5 parts of defoaming agent;
the gum dipping solution comprises the following components in parts by weight: 80-100 parts of thermosetting phenolic resin, 10-20 parts of PCTA copolymer, 2-5 parts of cross-linking agent, 8-15 parts of flame retardant, 25-30 parts of styrene-acrylic emulsion, 200-300 parts of methanol, 20-30 parts of isopropyl acetate and 2-5 parts of organic silanol sodium salt.
As a preferred aspect of the present invention, the composite wood pulp is made by the following process: mixing mercerized wood pulp and softwood pulp according to the mass ratio of 3-5: 1 to obtain mixed pulp, wherein the wood pulp concentration is 52.8-61.5 wt%, adding an aluminum sulfate solution and aluminum stearate to dissolve and mix uniformly, adjusting the pH value of the pulp to 3-5, heating to 75-80 ℃, slowly adding a calcium hydroxide emulsion under the stirring condition of 60-80 r/min, rapidly adding a titanate coupling agent and nano hydrotalcite powder, continuously stirring for 90-120 min, and standing to obtain the composite wood pulp.
In the invention, the mass of the added aluminum sulfate is 12-16 wt% of the mass of the mixed slurry, the molar ratio of the aluminum stearate, the calcium hydroxide and the aluminum sulfate is 0.1-0.2: 1.6-2: 1, and the mass ratio of the nano talcum powder, the titanium ester acid coupling agent and the aluminum sulfate is 0.3-0.5: 0.01-0.02: 1.
Preferably, the particle size of the nano hydrotalcite powder is 20 to 50 nm.
Preferably, the compatibilizer is a mixture of ethyl methacrylate and pyridine in a mass ratio of 1: 0.2-0.3.
Preferably, the defoaming agent is butanol or octanol.
Preferably, the flame retardant is a compound of melamine polyphosphate, polymethyl triethoxy silane and polyaluminium sulfate, and the mass ratio of the melamine polyphosphate, the polymethyl triethoxy silane and the polyaluminium sulfate is 2-3: 1-2: 1 in sequence.
The body of the base paper is prepared by taking composite wood pulp as a raw material and compounding the composite wood pulp with polyetherimide, polyethyleneimine and the like. The polyetherimide powder is an amorphous engineering resin, has flame retardant property and high temperature resistant dimensional stability, and plays a role in strengthening the heat resistant stability and the flame retardant property of the composite slurry. The melamine resin has waterproof performance, primary amine and secondary amine in the polyethyleneimine can perform cross-linking reaction with hydroxyl of wood pulp fiber, so that the dry strength of the filter paper is enhanced, and the flocculating effect and the filtering performance of the filter paper are enhanced.
Mercerized wood pulp in the composite wood pulp provides the bulk of the wood pulp fibers, while softwood pulp serves to strengthen the filter paper. The aluminum sulfate solution and the aluminum stearate solvent are firstly added into the slurry of the mercerized wood pulp and the softwood pulp to be uniform, then the calcium hydroxide emulsion is slowly added, the calcium hydroxide emulsion and the aluminum sulfate react to form network-shaped polymerized aluminum sulfate, and the aluminum stearate plays a stabilizing role. Because the main components of the wood pulp are porous cross-linked wood pulp fibers and a small amount of lignin, the polyaluminium sulfate is prepared in situ in the wood pulp by polymerization and forms an interpenetrating network structure with the wood pulp fibers. Polyaluminium sulfate is a flocculant commonly used in the process of treating wastewater in the paper industry, has a porous structure, and can be used as a filter medium. The inventor finds in practice that polyaluminium sulfate has high heat resistance and temperature resistance, and plays a role in modifying wood pulp fibers by forming interpenetrating network connection on the microstructure layer, so that the heat resistance and the temperature resistance of the wood pulp fibers can be enhanced. The polyaluminium sulfate can be decomposed to release crystal water when being heated at a high temperature of about 250 ℃, the surface temperature of the wood pulp fiber is reduced, the flame retardant effect is achieved, and the polyaluminium sulfate is decomposed at a higher temperature to obtain non-flammable substances such as aluminum oxide and the like, which are attached to the surface of the wood pulp fiber to achieve the oxygen-isolating flame retardant effect. Meanwhile, as the polyaluminium sulfate has a porous structure and has flocculation effect on small-particle-size impurities, the filtration and barrier efficiency of the prepared filter paper can be enhanced. After the calcium hydroxide emulsion is added, the interpenetrating network is not completely formed, nano hydrotalcite is added at the moment, the nano hydrotalcite can be stored in the interpenetrating network and is connected to the surface of wood pulp fibers through a titanate coupling agent, on one hand, the strength of the wood pulp fibers is enhanced, meanwhile, the water absorption performance of the hydrotalcite is weak, the waterproof performance of the wood pulp fibers is enhanced, on the other hand, the hydrotalcite can be heated and dehydrated at the temperature of 200 ℃ or above, particularly, the cooling flame-retardant effect of the polyaluminium sulfate is enhanced, meanwhile, carbonate contained in the hydrotalcite can be decomposed to generate carbon dioxide, the oxygen partial pressure is reduced, the oxygen-insulating flame-retardant effect is achieved, the hydrotalcite is converted into metal composite oxide, the strength is improved, and the heat-resistant.
The used compatibilizer is composed of ethyl methacrylate and pyridine according to the mass, can play a role in connection between wood pulp fibers, polyetherimide, melamine resin and the like, enhances the mixing uniformity of all components in the body of the base paper, and improves the performance of the filter paper, and the defoamer can be commonly used in papermaking, such as butanol, octanol and the like. The obtained filter paper body has high heat resistance and temperature resistance, and has better flame retardant property and use strength.
The thermosetting phenolic resin in the dipping solution plays a role in the thermosetting performance of the main body, and the PCTA copolymer is a polymer of cyclohexanedimethanol and terephthalic acid, has stronger heat resistance, impact resistance and chemical resistance, and improves the use strength and heat resistance of a cured layer after being compounded with the thermosetting phenolic resin. The flame retardant is obtained by compounding melamine polyphosphate, polymethyl triethoxy silane and polyaluminium sulfate according to a certain mass ratio. The inventor finds that the flame retardant effect of a single flame retardant is not ideal in practice, after melamine polyphosphate, polymethyltriethoxysilane and polyaluminium sulfate are compounded, polyaluminium sulfate is dispersed into thermosetting phenolic resin, the flame retardant effect of a gum dipping layer can be effectively enhanced through the flame retardant compounding effect of the melamine polyphosphate, the polymethyltriethoxysilane and the polyaluminium sulfate, methanol and isopropyl acetate play a role of a mixed solvent, and organosilicone sodium alkoxide enhances the hydrophobic and waterproof effects of the gum dipping layer.
The invention starts from two aspects of heat-resistant strength and flame-retardant property, by endowing the cured filter paper with stronger heat resistance and flame retardance and by the synergistic reinforcement of the heat resistance and the flame retardance, the obtained flame-retardant cured filter paper has strong flame retardance, high temperature resistance, high dimensional stability at high temperature, higher bursting strength and tearing strength and high filtering precision, and is suitable for being used as a filter element of an air filter of an engine.
The preparation method of the flame-retardant cured filter paper comprises the following steps:
(1) sequentially adding a succinimide ashless dispersant, a defoaming agent, melamine resin and a compatibilizer into the composite wood pulp liquid under the stirring condition, uniformly mixing, then adding polyetherimide powder, mixing, and adding polyethyleneimine to obtain a paper pulp stock solution;
(2) pulping the paper pulp stock solution, wherein the pulping degree is 32-40 DEG SR, obtaining a finished pulp with the pulp concentration of 1.82-2.11%, then performing net-surfing papermaking and squeezing dehydration under conventional conditions to obtain a base paper body, heating and keeping, and then placing at room temperature;
(3) putting thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and organosilicone sodium salt into a reaction kettle, stirring and mixing uniformly at 70-80 ℃, adding a flame retardant, mixing uniformly, adding a cross-linking agent and a PCTA copolymer, and mixing uniformly to obtain an impregnation solution; (4) and (3) placing the body of the base paper placed at room temperature obtained in the step (2) into an impregnation solution for impregnation, controlling the weight of the sizing material to be 17-18 wt%, and then heating and curing to obtain the flame-retardant cured filter paper.
Preferably, the heating temperature in the step (2) is 170-180 ℃, and the holding time is 60-90 min.
Preferably, the heating curing temperature in the step (4) is 140-150 ℃, and the curing time is 6-8 min.
The preparation method of the flame-retardant cured filter paper is based on the existing filter paper preparation process, firstly, the materials of the body of the base paper are mixed and pulped more pertinently, compared with the method of pulping the composite wood pulp liquid and then adding the compound materials, the uniform mixing of the pulp liquid is facilitated, meanwhile, the polyetherimide powder and the like can be fully contacted with the interpenetrating network structure in the composite wood pulp liquid, the pulping degree is strictly controlled in the pulping process, and the integrity of the interpenetrating network is kept. Heating the obtained base paper body at 170-180 ℃, on one hand, converting lignin in the wood pulp into a flowing state, promoting filling of hydrotalcite on generated pores, promoting partial glue solution components in the gum dipping process to be immersed, and enhancing the strength of the base paper body and the heat resistance in the using process, on the other hand, releasing free water between polyaluminium sulfate and hydrotalcite layers, and enhancing the dry strength of the base paper body. And then, taking out the base paper body after soaking in the dipping solution, heating and curing, so that the phenolic resin is fully crosslinked, and the glass state conversion of residual lignin in the base paper body is avoided, so that the cured filter paper has higher strength integrally. The gum applying amount of the gum dipping layer of the cured filter paper obtained by the method is reduced, the air permeability of the cured filter paper is enhanced, more importantly, the heat resistance of the cured filter paper is enhanced, and meanwhile, the preparation method omits the acid treatment process of wood pulp, has fewer steps, is concise in process and is easier to operate.
The invention has the following beneficial effects:
according to the invention, the cured filter paper is endowed with stronger heat resistance and flame retardance by matching the raw materials and the preparation method, and the heat resistance and the flame retardance are cooperatively enhanced, so that the filter paper has strong flame retardance, high temperature resistance and strong high-temperature dimensional stability, the strength and the filtering precision of the filter paper are high, the preparation method is less in steps, the process is simple, the operation is easier, and the obtained cured filter paper is suitable for being used as a filter element of an air filter of an engine.
Detailed Description
The following further describes the embodiments of the present invention.
The starting materials used in the present invention are commercially available or commonly used in the art, unless otherwise specified, and the methods in the following examples are conventional in the art, unless otherwise specified.
Example 1
The flame-retardant cured filter paper is prepared by taking out a base paper body after being soaked in a dipping solution and heating and curing, wherein:
the body of the base paper comprises the following components: 100g of composite wood pulp, 12g of polyetherimide powder, 4g of polyethyleneimine, 2g of melamine resin, 2g of compatibilizer, 4g of succinimide ashless dispersant and 2g of butanol, wherein the compatibilizer is a mixture of ethyl methacrylate and pyridine in a mass ratio of 1: 0.3;
the composite wood pulp is prepared by the following processes: mixing mercerized wood pulp and softwood pulp according to the mass ratio of 3:1 to obtain mixed pulp, adding an aluminum sulfate solution and aluminum stearate to dissolve and mix uniformly, wherein the mass of the aluminum sulfate is 12 wt% of the mass of the mixed pulp, adjusting the pH value of the pulp to 5 by using sulfuric acid, heating to 75 ℃, slowly adding a calcium hydroxide emulsion under the stirring condition of 60r/min, the molar ratio of the aluminum stearate to the calcium hydroxide to the aluminum sulfate is 0.1:1.6:1, rapidly adding a titanium ester acid coupling agent and nano hydrotalcite powder, the mass ratio of the nano talcum powder to the titanium ester acid coupling agent to the aluminum sulfate is 0.3:0.01:1, the particle size range of the nano hydrotalcite powder is 20-50 nm, continuously stirring for 90min, and standing to obtain composite wood pulp;
the gum dipping solution consists of the following components: 80g of thermosetting phenolic resin, 10g of PCTA copolymer, 2g of cross-linking agent, 8g of flame retardant, 25g of styrene-acrylic emulsion, 200g of methanol, 20g of isopropyl acetate and 2g of sodium organosiliconate; the flame retardant is a compound consisting of melamine polyphosphate, polymethyl triethoxy silane and polyaluminium sulfate according to the mass ratio of 2:1: 1.
The preparation method of the flame-retardant cured filter paper comprises the following steps:
(1) sequentially adding a succinimide ashless dispersant, a defoaming agent, melamine resin and a compatibilizer into the composite wood pulp liquid under the stirring condition, uniformly mixing, then adding polyetherimide powder, mixing, and adding polyethyleneimine to obtain a paper pulp stock solution;
(2) pulping the paper pulp stock solution, wherein the pulping degree is 32 DEG SR, obtaining finished pulp with the pulp concentration of 1.82%, then performing net-surfing papermaking and squeezing dehydration under conventional conditions to obtain a base paper body, heating to 170 ℃, keeping for 90min, and then placing at room temperature;
(3) putting thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and organosilicone sodium salt into a reaction kettle, stirring and mixing uniformly at 70 ℃, adding a flame retardant, mixing uniformly, adding a cross-linking agent and a PCTA copolymer, and mixing uniformly to obtain an impregnation solution;
(4) and (3) placing the body of the base paper placed at room temperature obtained in the step (2) into a dipping solution for dipping, controlling the sizing material to be 17 wt%, and then heating to 140 ℃ for curing for 8min to obtain the flame-retardant cured filter paper.
Example 2
The flame-retardant cured filter paper is prepared by taking out a base paper body after being soaked in a dipping solution and heating and curing, wherein:
the body of the base paper comprises the following components: 120g of composite wood pulp, 16g of polyetherimide powder, 5g of polyethyleneimine, 4g of melamine resin, 4g of compatibilizer, 5g of succinimide ashless dispersant and 5g of butanol, wherein the compatibilizer is a mixture of ethyl methacrylate and pyridine in a mass ratio of 1: 0.2;
the composite wood pulp is prepared by the following processes: mixing mercerized wood pulp and softwood pulp according to a mass ratio of 4:1 to obtain mixed pulp, adding an aluminum sulfate solution and aluminum stearate to dissolve and mix uniformly, wherein the mass of the aluminum sulfate is 14 wt% of the mass of the mixed pulp, adjusting the pH value of the pulp to 4 by using sulfuric acid, heating to 78 ℃, slowly adding a calcium hydroxide emulsion under the stirring condition of 70r/min, the molar ratio of the aluminum stearate to the calcium hydroxide to the aluminum sulfate is 0.2:1.8:1, rapidly adding a titanium ester acid coupling agent and nano hydrotalcite powder, the mass ratio of the nano talcum powder to the titanium ester acid coupling agent to the aluminum sulfate is 0.4:0.01:1, the particle size range of the nano hydrotalcite powder is 20-50 nm, continuously stirring for 100min, and standing to obtain composite wood pulp;
the gum dipping solution consists of the following components: 90g of thermosetting phenolic resin, 15g of PCTA copolymer, 4g of cross-linking agent, 12g of flame retardant, 27g of styrene-acrylic emulsion, 250g of methanol, 25g of isopropyl acetate and 4g of sodium organosiliconate; the flame retardant is a compound consisting of melamine polyphosphate, polymethyl triethoxy silane and polyaluminium sulfate according to the mass ratio of 2:2: 1.
The preparation method of the flame-retardant cured filter paper comprises the following steps:
(1) sequentially adding a succinimide ashless dispersant, a defoaming agent, melamine resin and a compatibilizer into the composite wood pulp liquid under the stirring condition, uniformly mixing, then adding polyetherimide powder, mixing, and adding polyethyleneimine to obtain a paper pulp stock solution;
(2) pulping the paper pulp stock solution, wherein the pulping degree is 37 DEG SR, obtaining finished pulp with the pulp concentration of 2.01 percent, then performing net-surfing papermaking and squeezing dehydration under the conventional conditions to obtain a base paper body, heating to 175 ℃, keeping for 80min, and then placing at room temperature;
(3) putting thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and organosilicone sodium salt into a reaction kettle, stirring and mixing uniformly at 75 ℃, adding a flame retardant, mixing uniformly, adding a cross-linking agent and a PCTA copolymer, and mixing uniformly to obtain an impregnation solution;
(4) and (3) placing the body of the base paper placed at room temperature obtained in the step (2) into a dipping solution for dipping, controlling the sizing material to be 17 wt%, and then heating to 145 ℃ for curing for 7min to obtain the flame-retardant cured filter paper.
Example 3
The flame-retardant cured filter paper is prepared by taking out a base paper body after being soaked in a dipping solution and heating and curing, wherein:
the body of the base paper comprises the following components: 110g of composite wood pulp, 20g of polyetherimide powder, 3g of polyethyleneimine, 3g of melamine resin, 5g of compatibilizer, 6g of succinimide ashless dispersant and 3g of octanol, wherein the compatibilizer is a mixture of ethyl methacrylate and pyridine in a mass ratio of 1: 0.27;
the composite wood pulp is prepared by the following processes: mixing mercerized wood pulp and softwood pulp according to the mass ratio of 5:1 to obtain mixed pulp, adding an aluminum sulfate solution and aluminum stearate to dissolve and mix uniformly, wherein the mass of the aluminum sulfate is 16wt% of the mass of the mixed pulp, adjusting the pH value of the pulp to 3 by using sulfuric acid, heating to 80 ℃, slowly adding a calcium hydroxide emulsion under the stirring condition of 80r/min, the molar ratio of the aluminum stearate to the calcium hydroxide to the aluminum sulfate is 0.15:2:1, rapidly adding a titanium ester acid coupling agent and nano hydrotalcite powder, the mass ratio of the nano talcum powder to the titanium ester acid coupling agent to the aluminum sulfate is 0.5:0.02:1, the particle size range of the nano hydrotalcite powder is 20-50 nm, continuously stirring for 120min, and standing to obtain composite wood pulp;
the gum dipping solution consists of the following components: 100g of thermosetting phenolic resin, 20g of PCTA copolymer, 5g of cross-linking agent, 15g of flame retardant, 30g of styrene-acrylic emulsion, 300g of methanol, 30g of isopropyl acetate and 5g of sodium organosiliconate; the flame retardant is a compound consisting of melamine polyphosphate, polymethyl triethoxy silane and polyaluminium sulfate according to the mass ratio of 3:1: 1.
The preparation method of the flame-retardant cured filter paper comprises the following steps:
(1) sequentially adding a succinimide ashless dispersant, a defoaming agent, melamine resin and a compatibilizer into the composite wood pulp liquid under the stirring condition, uniformly mixing, then adding polyetherimide powder, mixing, and adding polyethyleneimine to obtain a paper pulp stock solution;
(2) pulping the paper pulp stock solution, wherein the pulping degree is 40 DEG SR, obtaining finished pulp with the pulp concentration of 2.11%, then performing net-surfing papermaking and squeezing dehydration under conventional conditions to obtain a base paper body, heating to 180 ℃, keeping for 60min, and then placing at room temperature;
(3) putting thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and organosilicone sodium salt into a reaction kettle, stirring and mixing uniformly at 80 ℃, adding a flame retardant, mixing uniformly, adding a cross-linking agent and a PCTA copolymer, and mixing uniformly to obtain an impregnation solution;
(4) and (3) placing the body of the base paper placed at room temperature obtained in the step (2) into a dipping solution for dipping, controlling the sizing material to be 18wt%, and then heating to 150 ℃ for curing for 6min to obtain the flame-retardant cured filter paper.
Comparative example 1
The method and raw material preparation according to example 1 were carried out, except for example 1, in which the composite wood pulp in the raw material was prepared by directly adding polymeric aluminum sulfate to the mixed pulp of mercerized wood pulp and softwood pulp in an amount of 20 wt% based on the mass of the mixed pulp.
Comparative example 2
According to the method and raw material preparation of the embodiment 1, the difference from the embodiment 1 is that in the preparation process of the base paper body, the composite wood pulp is beaten according to the method of the step (2), then the raw materials except the composite wood pulp in the step (1) are added into the beaten composite wood pulp to be mixed to obtain the pulp stock solution, and then the pulp stock solution is made into paper and pressed to obtain the base paper body.
Comparative example 3
According to the method and raw material preparation of the example 1, the difference from the example 1 is that in the preparation process of the base paper body, the base paper body obtained in the step (2) is directly soaked in the soaking solution under the condition of not heating and keeping, and is taken out and heated and cured for 8min at 150 ℃.
Comparative example 4
The method and the raw material preparation according to example 1 differ from example 1 in that the same amount of melamine polyphosphate is used as the flame retardant during the preparation of the impregnation liquor.
Comparative example 5
The method and the raw material preparation according to the example 1 are different from the example 1 in that the flame retardant used in the preparation of the impregnating solution is a mixture of melamine polyphosphate and polymethyltriethoxysilane in the same amount, and the mass ratio of the melamine polyphosphate to the polymethyltriethoxysilane is 2:1.
The performance indexes such as strength and air permeability of the cured filter paper obtained in each of the above examples and comparative examples and the results of the flame retardant performance indexes measured with reference to GB/T14656-2009 "flame retardant paper and paperboard burning performance test method" are shown in table 1, wherein when testing bursting strength and stiffness, the cured filter paper to be tested is first placed in an oven at 180 ℃ and then subjected to heat preservation for 60 min.
Claims (9)
1. The flame-retardant cured filter paper is characterized by being prepared by taking out a base paper body after the base paper body is soaked in a dipping solution and heating and curing, wherein:
the body of the base paper comprises the following components in parts by weight: 100-120 parts of composite wood pulp, 12-20 parts of polyetherimide powder, 3-5 parts of polyethyleneimine, 2-4 parts of melamine resin, 2-5 parts of compatibilizer, 4-6 parts of succinimide ashless dispersant and 2-5 parts of defoaming agent;
the gum dipping solution comprises the following components in parts by weight: 80-100 parts of thermosetting phenolic resin, 10-20 parts of PCTA copolymer, 2-5 parts of cross-linking agent, 8-15 parts of flame retardant, 25-30 parts of styrene-acrylic emulsion, 200-300 parts of methanol, 20-30 parts of isopropyl acetate and 2-5 parts of sodium organosiliconate;
the composite wood pulp is prepared by the following processes: mixing mercerized wood pulp and softwood pulp according to the mass ratio of 3-5: 1 to obtain mixed pulp, wherein the wood pulp concentration is 52.8-61.5 wt%, adding an aluminum sulfate solution and aluminum stearate to dissolve and mix uniformly, adjusting the pH value of the pulp to 3-5, heating to 75-80 ℃, slowly adding a calcium hydroxide emulsion under the stirring condition of 60-80 r/min, rapidly adding a titanate coupling agent and nano hydrotalcite powder, continuously stirring for 90-120 min, and standing to obtain the composite wood pulp.
2. The flame-retardant cured filter paper as claimed in claim 1, wherein the mass of the added aluminum sulfate is 12-16 wt% of the mass of the mixed slurry, the molar ratio of the aluminum stearate, the calcium hydroxide and the aluminum sulfate is 0.1-0.2: 1.6-2: 1, and the mass ratio of the nano hydrotalcite powder, the titanate coupling agent and the aluminum sulfate is 0.3-0.5: 0.01-0.02: 1.
3. The flame retardant cured filter paper as recited in claim 1, wherein the nano hydrotalcite powder has a particle size of 20 to 50 nm.
4. The flame-retardant cured filter paper as recited in claim 1, wherein the compatibilizer is a mixture of ethyl methacrylate and pyridine in a mass ratio of 1: 0.2-0.3.
5. The flame retardant cured filter paper of claim 1, wherein the defoamer is butanol or octanol.
6. The flame-retardant cured filter paper as claimed in claim 1, wherein the flame retardant is a compound of melamine polyphosphate, polymethyltriethoxysilane and polyaluminium sulfate, and the mass ratio of the melamine polyphosphate, the polymethyltriethoxysilane and the polyaluminium sulfate is 2-3: 1-2: 1 in sequence.
7. The method of making flame retardant cured filter paper according to any of claims 1 to 6, comprising the steps of:
(1) sequentially adding a succinimide ashless dispersant, a defoaming agent, melamine resin and a compatibilizer into the composite wood pulp liquid under the stirring condition, uniformly mixing, then adding polyetherimide powder, mixing, and adding polyethyleneimine to obtain a paper pulp stock solution;
(2) pulping the paper pulp stock solution, wherein the pulping degree is 32-40 DEG SR, obtaining a finished pulp with the pulp concentration of 1.82-2.11%, then performing net-surfing papermaking and squeezing dehydration under conventional conditions to obtain a base paper body, heating and keeping, and then placing at room temperature;
(3) putting thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and organosilicone sodium salt into a reaction kettle, stirring and mixing uniformly at 70-80 ℃, adding a flame retardant, mixing uniformly, adding a cross-linking agent and a PCTA copolymer, and mixing uniformly to obtain an impregnation solution;
(4) and (3) placing the body of the base paper placed at room temperature in the step (2) into a dipping solution for dipping, controlling the weight of the sizing material to be 17-18 wt%, and then heating and curing to obtain the flame-retardant cured filter paper.
8. The method for preparing the flame-retardant cured filter paper according to claim 7, wherein the heating temperature in the step (2) is 170-180 ℃, and the holding time is 60-90 min.
9. The preparation method of the flame-retardant cured filter paper as claimed in claim 7, wherein the heating curing temperature in the step (4) is 140-150 ℃, and the curing time is 6-8 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811376775.3A CN109610238B (en) | 2018-11-19 | 2018-11-19 | Flame-retardant cured filter paper and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811376775.3A CN109610238B (en) | 2018-11-19 | 2018-11-19 | Flame-retardant cured filter paper and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109610238A CN109610238A (en) | 2019-04-12 |
| CN109610238B true CN109610238B (en) | 2021-04-09 |
Family
ID=66004438
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811376775.3A Active CN109610238B (en) | 2018-11-19 | 2018-11-19 | Flame-retardant cured filter paper and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109610238B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113789686A (en) * | 2021-07-23 | 2021-12-14 | 天津科技大学 | High-temperature-resistant engine oil filter paper and preparation method thereof |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI417329B (en) * | 2008-07-18 | 2013-12-01 | Ticona Llc | Flame retardant polymer composition |
| CN102618360B (en) * | 2011-01-27 | 2014-06-04 | 中国石油化工股份有限公司 | Compressor oil composition |
| CN102912677B (en) * | 2012-09-20 | 2015-12-02 | 安徽凤凰滤清器股份有限公司 | A kind of filter of automobile engine air paper and preparation method thereof |
| CN104894913A (en) * | 2015-05-11 | 2015-09-09 | 杭州特种纸业有限公司 | Flame-retardant air filter paper, preparation method therefor and application thereof |
| CN104831586B (en) * | 2015-05-11 | 2016-06-08 | 杭州特种纸业有限公司 | Heavy load curing oil filter paper and its preparation method and application |
| CN106567288A (en) * | 2016-11-14 | 2017-04-19 | 蚌埠市风驰滤清器有限公司 | Filter paper with high dust containing capacity for filter |
-
2018
- 2018-11-19 CN CN201811376775.3A patent/CN109610238B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN109610238A (en) | 2019-04-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| WO2022057467A1 (en) | Modified collagen fiber and use thereof | |
| CN102899969B (en) | High-temperature and corrosion resistant filter paper for fuel filter and preparation method thereof | |
| CN109610238B (en) | Flame-retardant cured filter paper and preparation method thereof | |
| JPS599300A (en) | Paper cover sheet for gypsum board, production thereof and produced gypsum board | |
| CN109653024A (en) | A kind of single side applies solidification filter paper and preparation method thereof | |
| CN105568769A (en) | Diesel filter paper and preparation method thereof | |
| CN105714597A (en) | Engine oil filter paper and preparation method thereof | |
| AU2014257876A1 (en) | Process for the treatment of cellulose fibers | |
| CN109159226A (en) | A kind of method of inorganic coagulation material strengthened artificial forest timber | |
| CN108752980A (en) | The preparation method of modified magnesium hydroxide flame retardant agent and modified magnesium hydroxide flame retardant agent | |
| CN109518530B (en) | Laminated thick vulcanized paper and preparation method thereof | |
| CN111218853A (en) | Paper-based functional material for oil-water separation and preparation method and application thereof | |
| CN108103832A (en) | A kind of photochromic speciality paper and preparation method thereof | |
| CN105986528A (en) | Hydraulic oil filter paper capable of separating oil from water efficiently | |
| CN108529633B (en) | Method for recycling white carbon black with high oil absorption value from optical rod waste with low equipment corrosivity | |
| CN105986520A (en) | Mixed filler added filter paper for hydraulic filter | |
| CN107326728B (en) | A kind of red grinding vulcan fibre of strong coloring force | |
| CN112372774B (en) | Bamboo-based fiber composite material and continuous preparation method thereof | |
| DK168482B1 (en) | Aqueous amine resin composition, process for its preparation, binder for mineral fibers containing such composition, and process for preparing an insulating material | |
| EP3625185A1 (en) | Cellulose filaments reinforced cement composite board and method for the manufacture of the same | |
| CN109338809A (en) | A kind of water-fast thick vulcan fibre and preparation method thereof | |
| CN115849823B (en) | Color calcium silicate board substrate and preparation method and application thereof | |
| CN105986527A (en) | Hydraulic filter filtering paper with modified rosin for water resistance improvement | |
| CN115162054B (en) | Waterproof engine oil filter paper and preparation method thereof | |
| JPS5971498A (en) | Aluminum hydroxide contained paper and production thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Flame retardant solidified filter paper and its preparation method Effective date of registration: 20221014 Granted publication date: 20210409 Pledgee: Hengfeng Bank Co.,Ltd. Hangzhou Fuyang sub branch Pledgor: HANGZHOU SPECIAL PAPER Co.,Ltd. Registration number: Y2022980018349 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |