CN109610238A - Fire-retardant solidification filter paper of one kind and preparation method thereof - Google Patents
Fire-retardant solidification filter paper of one kind and preparation method thereof Download PDFInfo
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- CN109610238A CN109610238A CN201811376775.3A CN201811376775A CN109610238A CN 109610238 A CN109610238 A CN 109610238A CN 201811376775 A CN201811376775 A CN 201811376775A CN 109610238 A CN109610238 A CN 109610238A
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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
- 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
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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
- D21H17/54—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
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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
- 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
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Abstract
The present invention relates to solidification filter paper technical fields, for the flame retardant property for improving filter paper, meet the application demand of filter paper on the engine, the present invention provides fire-retardant solidification filter paper of one kind and preparation method thereof, the fire-retardant solidification filter paper takes out to be heating and curing and be made after being impregnated in dipping solution by body paper ontology, wherein body paper ontology is by compound wood pulp liquid, polyetherimide powder, polyethyleneimine, melamine resin, expanding material, Ashless butyl diimide dispersant and defoaming agent are made, dipping solution is by thermosetting phenolic resin, PCTA copolymer, crosslinking agent, fire retardant, styrene-acrylic emulsion, methanol, isopropyl acetate and Organosilicon Alcohol in Organic sodium salt are made.The flame retardant property of fire-retardant solidification filter paper of the invention is strong, high temperature resistant, and high temperature dimensional stability is strong, and the intensity of filter paper and filtering accuracy are high, it is few that preparation method saves step, process is succinct, is more easier to operate, and the filter core that gained solidifies the air cleaner that filter paper is suitable as engine uses.
Description
Technical field
The present invention relates to solidification filter paper technical fields, and in particular to fire-retardant solidification filter paper of one kind and preparation method thereof.
Background technique
Air cleaner is located in the gas handling system of engine, is mounted on the front of automobile carburetor or air inlet pipe, plays
The effect of dust in air, sand grains is filtered out, guarantees to enter enough, clean air in cylinder.Common air cleaner has used
Property oil bath air cleaner, papery dry-type air cleaner, polyurethane filter-element air filter etc..Wherein papery dry air
The micropore filter paper that the filter core of filter is handled by adhesive is made, and adhesive forms the cured layer of filter core, and micropore filter paper is then main
It is manufactured paper with pulp and is made by plant fibre slurry liquid, had the advantages that filtering efficiency is high, structure is simple, light weight and cost is low etc., be to apply at present
Relatively broad air filter for automobile.But because micropore filter paper has inflammability, the appearance when cylinder is tempered
Also the burning that can cause paper filter core when easily causing filter core to burn, while having combustibles in the air of engine sucking, influences
Traffic safety, therefore it is required that filter paper has certain flame retardant property.And due to the high-temperature work environment of engine, filter is also required
Paper has certain heat-resisting quantity.
Chinese patent CN201521054157.9, patent name " a kind of flame retardant filter paper " disclose one kind by first filter layer, essence
Filtering layer and penetrated into from first filter layer upper surface filter bed of essence lower surface flame-retardant layer flame retardant filter paper, between first filter layer and filter bed of essence
Flame-retardant layer is set, which is made of halogen-free flame retardants, provides filter paper flame retardant property.But since flame retardant effect is derived only from
The resistance to combustion of flame-retardant layer, first filter layer and filter bed of essence and heat resistance are general, therefore the whole flame retardant property of filter paper is still to be improved.
Summary of the invention
For the flame retardant property for improving filter paper, meet the application demand of filter paper on the engine, it is an object of the invention to mention
For a kind of fire-retardant solidification filter paper, there is stronger flame retardant property, and high temperature resistance is stronger, is suitable as the air of engine
The filter core of filter uses.
Another object of the present invention is to provide the fire-retardant preparation methods for solidifying filter paper.
The present invention provides the following technical solution:
A kind of fire-retardant solidification filter paper, taking-up, which is heating and curing, after being impregnated in dipping solution by body paper ontology is made, in which:
Body paper ontology is made of the component of following parts by weight: 100~120 parts of compound wood pulp liquid, polyetherimide powder 12~20
Part, 3~5 parts of polyethyleneimine, 2~4 parts of melamine resin, 2~5 parts of expanding material, Ashless butyl diimide dispersant 4~6
Part, 2~5 parts of defoaming agent；
Dipping solution is made of the component of following parts by weight: 80~100 parts of thermosetting phenolic resin, 0~20 part of PCTA copolymer 1,
2~5 parts of crosslinking agent, 8~15 parts of fire retardant, 25~30 parts of styrene-acrylic emulsion, 200~300 parts of methanol, isopropyl acetate 20~30
Part, 2~5 parts of Organosilicon Alcohol in Organic sodium salt.
As a preference of the present invention, the compound wood pulp liquid is made of following procedure: by mercerization wood pulp and softwood pulp
3~5:1 in mass ratio mixes to obtain mixed serum, and wood pulp concentration is 52.8~61.5wt%, and aluminum sulfate solution and stearic acid is added
Aluminium dissolution is uniformly mixed, and adjusts the pH value of slurries to 3~5, is then heated to 75~80 DEG C, under 60~80r/min stirring condition
Be slowly added to calcium hydroxide emulsion, then investment titanium esters acid coupling agent, nano hydrotalcite powder rapidly, then proceed to stirring 90~
120min stands to obtain compound wood pulp liquid.
As a preference of the present invention, the quality for the aluminum sulfate being added is 12~16wt% of mixed serum quality, stearic acid
The molar ratio of aluminium, calcium hydroxide and aluminum sulfate is 0.1~0.2:1.6~2:1, nano talc, titanium esters acid coupling agent and sulfuric acid
The mass ratio of aluminium is 0.3~0.5:0.01~0.02:1.
As a preference of the present invention, the particle size range of the nano hydrotalcite powder is 20~50nm.
As a preference of the present invention, expanding material is the mixing of ethyl methacrylate and pyridine 1:0.2~0.3 in mass ratio
Object.
As a preference of the present invention, the defoaming agent is butanol or octanol.
As a preference of the present invention, the fire retardant be Melamine Polyphosphate, poly- methyltriethoxysilane with
The compound of polyaluminium sulfate, the mass ratio of three are followed successively by 2~3:1~2:1.
Body paper ontology of the invention is using compound wood pulp liquid as raw material, by compounding with polyetherimide, polyethyleneimine etc.
It is made.Polyetherimide powder is a kind of unformed engineering resin, has flame retardant property and high temperature resistant dimensional stability, plays
Strengthen the heat-resistant stability of compound slurry and the effect of flame retardant property.Melamine resin plays waterproof performance, polyethyleneimine
In primary amine and secondary amine can crosslink and react with the hydroxyl of wood pulp cellulose, enhance the dry strength of filter paper, and wadding can be played
Solidifying effect, strengthens the strainability of filter paper.
The wood pulp cellulose of mercerization wood pulp provider in compound wood pulp liquid, and softwood pulp plays and strengthens filter paper intensity
Effect.To being firstly added aluminum sulfate solution in the slurries of mercerization wood pulp and softwood pulp and aluminum stearate solvent is uniform, then
It is slowly added to calcium hydroxide emulsion, calcium hydroxide emulsion and reacting aluminum sulfate form network-like polyaluminium sulfate, aluminum stearate
Play stabilization.Since the main component of wood pulp is the wood pulp cellulose and a small amount of lignin of cavernous crosslinking,
Polyaluminium sulfate in-situ polymerization in wood pulp prepares and forms inierpeneirating network structure with wood pulp cellulose.Polyaluminium sulfate is paper maker
Common flocculant in industry wastewater treatment process has porous structure, can be used as filter medium use.Inventor is in practice
It was found that polyaluminium sulfate has stronger heat-resisting and heat resistance, by forming interpenetrating networks connection in microstructure level, rise
To the modifying function to wood pulp cellulose, heat-resisting, the heat resistance of wood pulp cellulose can be enhanced.Polyaluminium sulfate is at 250 DEG C or so
It can be decomposed when high-temperature heating and release the crystallization water, reduce wood pulp cellulose surface temperature, and play fire retardation, and higher
At a temperature of polyaluminium sulfate decompose to obtain the non-flammable substance such as aluminium oxide, be attached to wood pulp cellulose surface, play oxygen barrier fire-retardant effect
Fruit.Simultaneously as polyaluminium sulfate itself has porous structure, and there is flocculation to small particle impurity, therefore can be strong
Change the filtering barriering efficiency of the filter paper of preparation.After calcium hydroxide emulsion is added, interpenetrating networks not yet form completely, at this time
Nano hydrotalcite is added, can be stored in interpenetrating networks, and be connected to wood pulp cellulose surface through titanium esters acid coupling agent, on the one hand
Enhance the intensity of wood pulp cellulose, while hydrotalcite water absorbing properties are weak, enhance the waterproof performance of wood pulp cellulose, another aspect hydrotalcite
200 DEG C of front and backs, can especially be heated at 250 DEG C or more dehydration, strengthen the cooling flame retardant effect of polyaluminium sulfate, while neatly
The carbonate contained in stone can decompose generation carbon dioxide, reduce partial pressure of oxygen, play oxygen barrier flame retardant effect, and hydrotalcite then changes
For composite oxide of metal, intensity gets a promotion, and improves the high-temperature capability of wood pulp cellulose at high temperature.
Expanding material used is made of ethyl methacrylate and pyridine by quality, can be in wood pulp cellulose and polyetherimide
Connection function is played between amine, melamine resin etc., enhances the mixing uniformity of each component in body paper ontology, improves filter paper
Can, defoaming agent can be common defoaming agent in papermaking, such as butanol, octanol.Heat-resisting, the temperature tolerance of gained filter paper ontology in this way
Can be high, and there is preferable flame retardant property and use intensity.
Thermosetting phenolic resin in dipping solution plays the Thermocurable energy of main body, and PCTA copolymer is hexamethylene diformazan
The polymer of pure and mild terephthalic acids has stronger heat resistance, shock resistance and chemical-resistance, with thermosetting phenolic resin
Use intensity, the heat resistance of cured layer are improved after compounding.Fire retardant is by Melamine Polyphosphate, poly- methyl triethoxy
Silane compounds to obtain according to a certain mass ratio with polyaluminium sulfate.Inventor is in practice, it has been found that single fire retardant added
Flame retardant effect is not satisfactory, and after Melamine Polyphosphate, poly- methyltriethoxysilane are compounded with polyaluminium sulfate,
It is distributed in thermosetting phenolic resin using polyaluminium sulfate, passes through Melamine Polyphosphate, poly- methyltriethoxy silane
The fire-retardant complex role of alkane and polyaluminium sulfate can effectively enhance the flame retardant effect of rubber shoe latex layer, and methanol and isopropyl acetate play
The effect of mixed solvent, Organosilicon Alcohol in Organic sodium salt then enhance the hydrophobic of rubber shoe latex layer, waterproof effect.
The present invention starts in terms of high-temperature capability and flame retardant property two, by assigning the stronger heat resistance of solidification filter paper and resistance
Combustion property, and by heat resistance and flame retardant type phase cooperative reinforcing, the flame retardant property that obtained flame-retardant solidifies filter paper is strong, high temperature resistant, high temperature
Under dimensional stability it is high, while bursting strength with higher and tearability, filtering accuracy is high, is suitable as the air of engine
The filter core of filter uses.
The above-mentioned fire-retardant preparation method for solidifying filter paper, comprising the following steps:
(1) Ashless butyl diimide dispersant, defoaming agent, melamine tree are sequentially added under stirring condition into compound wood pulp liquid
Rouge and expanding material are uniformly mixed, and polyetherimide powder mixing is then added, adds polyethyleneimine and obtains paper pulp stoste；
(2) paper pulp stoste is beaten, beating degree is 32~40 ° of SR, and obtaining slurry concentration is 1.82~2.11% to be slurried, then
Normal condition online is manufactured paper with pulp, press dewatering obtains body paper ontology, and then heating keeps being placed on being placed at room temperature for；
(3) thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and Organosilicon Alcohol in Organic sodium salt are placed in 70 in reaction kettle
~80 DEG C are uniformly mixed, and are added after fire retardant mixes and add crosslinking agent, PCTA copolymer is uniformly mixed and obtains maceration extract；
(4) the body paper ontology being placed at room temperature for obtained by step (2) is placed in maceration extract and is impregnated, sizing material is 17~18wt% in control, so
After be heating and curing, obtain fire-retardant solidification filter paper.
As the preferred of the method for the present invention, heating temperature is 170~180 DEG C in step (2), 60~90min of retention time.
As the preferred of the method for the present invention, the temperature that is heating and curing of step (4) is 140~150 DEG C, curing time 6~
8min。
Fire-retardant solidification filter paper preparation method of the invention is on the basis of existing filter paper preparation process, more first
The material of body paper ontology is mixed with beating, compared with being individually beaten compound wood pulp liquid and compounding material is then added, is conducive to starch
Liquid is uniformly mixed, while polyetherimide powder etc. can be contacted sufficiently with the inierpeneirating network structure in compound wood pulp liquid, and
The strict control beating degree in pulping process keeps the integrality of interpenetrating networks.By obtained body paper ontology at 170~180 DEG C
On the one hand lignin conversion in wood pulp liquid is promoted filling of the hydrotalcite to the hole of generation at flowable state, and promoted by lower heating
It is immersed into the part glue component in immersing glue process, enhances the intensity of body paper ontology and the heat resistance of use process, on the other hand
It is released the free water of polyaluminium sulfate and hydrotalcite layers, enhances the stemness intensity of body paper ontology.Then by body paper
Ontology takes out after impregnating in dipping solution and is heating and curing, and on the one hand makes phenolic resin full cross-linked, on the other hand avoids body paper sheet
The glass transition of residual lignin in body makes to solidify filter paper integrally intensity with higher.It is resulting by the method for the invention
The spread for solidifying the rubber shoe latex layer of filter paper is reduced, and solidifies the permeability enhancing of filter paper, and more importantly enhances solidification
The heat resistance of filter paper, while the sour treatment process of wood pulp is omitted in preparation method, step is few, and process is succinct, is more easier to operate.
Beneficial effects of the present invention are as follows:
Cooperation assigns the stronger heat resistance of solidification filter paper and anti-flammability in terms of the present invention passes through raw material and preparation method two, and passes through
Heat resistance and flame retardant type phase cooperative reinforcing, make that the flame retardant property of filter paper is strong, high temperature resistant, and high temperature dimensional stability is strong, and filter paper
Intensity and filtering accuracy it is high, preparation method saves that step is few, and process is succinct, is more easier to operate, gained solidification filter paper is suitable for
Filter core for the air cleaner of engine uses.
Specific embodiment
A specific embodiment of the invention is described further below.
Unless otherwise instructed, raw material employed in the present invention is commercially available or commonly used in the art, such as
Without special instruction, the method in following embodiments is the conventional method of this field.
Embodiment 1
A kind of fire-retardant solidification filter paper, taking-up, which is heating and curing, after being impregnated in dipping solution by body paper ontology is made, in which:
Body paper ontology is made of the following components: compound wood pulp liquid 100g, polyetherimide powder 12g, polyethyleneimine 4g, trimerization
Melamine resin 2g, expanding material 2g, Ashless butyl diimide dispersant 4g, butanol 2g, expanding material are ethyl methacrylate and pyrrole
The pyridine mixture of 1:0.3 in mass ratio；
Compound wood pulp liquid is made of following procedure: mercerization wood pulp and softwood pulp 3:1 in mass ratio are mixed into obtain mixed serum,
Wood pulp concentration is 52.8wt%, and aluminum sulfate solution is added and aluminum stearate dissolution is uniformly mixed, the quality of aluminum sulfate is mixing slurry
The 12wt% of liquid quality, the pH value for adjusting slurries with sulfuric acid are then heated to 75 DEG C, slowly add under 60r/min stirring condition to 5
Enter calcium hydroxide emulsion, the molar ratio of aluminum stearate, calcium hydroxide and aluminum sulfate is 0.1:1.6:1, then investment titanium esters acid rapidly
The mass ratio of coupling agent, nano hydrotalcite powder, nano talc, titanium esters acid coupling agent and aluminum sulfate is 0.3:0.01:1, is received
The particle size range of rice hydrotalcite powder is 20~50nm, then proceedes to stirring 90min, stands to obtain compound wood pulp liquid；
Dipping solution is made of the following components: thermosetting phenolic resin 80g, PCTA copolymer 1 0g, crosslinking agent 2g, fire retardant 8g, benzene
Acrylic emulsion 25g, methanol 200g, isopropyl acetate 20g, Organosilicon Alcohol in Organic sodium salt 2g；Fire retardant is Melamine Polyphosphate, gathers
The compound of methyltriethoxysilane and polyaluminium sulfate 2:1:1 in mass ratio composition.
The above-mentioned fire-retardant preparation method for solidifying filter paper, comprising the following steps:
(1) Ashless butyl diimide dispersant, defoaming agent, melamine tree are sequentially added under stirring condition into compound wood pulp liquid
Rouge and expanding material are uniformly mixed, and polyetherimide powder mixing is then added, adds polyethyleneimine and obtains paper pulp stoste；
(2) paper pulp stoste is beaten, beating degree is 32 ° of SR, and obtaining slurry concentration is 1.82% to be slurried, then in normal condition
Net is manufactured paper with pulp, press dewatering obtains body paper ontology, is heated to 170 DEG C of holding 90min, is subsequently placed in and is placed at room temperature for；
(3) thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and Organosilicon Alcohol in Organic sodium salt are placed in 70 in reaction kettle
It DEG C is uniformly mixed, is added after fire retardant mixes and adds crosslinking agent, PCTA copolymer is uniformly mixed and obtains maceration extract；
(4) the body paper ontology being placed at room temperature for obtained by step (2) is placed in maceration extract and is impregnated, sizing material is 17wt% in control, so
After be heated to 140 DEG C of solidification 8min, obtain fire-retardant solidification filter paper.
Embodiment 2
A kind of fire-retardant solidification filter paper, taking-up, which is heating and curing, after being impregnated in dipping solution by body paper ontology is made, in which:
Body paper ontology is made of the following components: compound wood pulp liquid 120g, polyetherimide powder 16g, polyethyleneimine 5g, trimerization
Melamine resin 4g, expanding material 4g, Ashless butyl diimide dispersant 5g, butanol 5g, expanding material are ethyl methacrylate and pyrrole
The pyridine mixture of 1:0.2 in mass ratio；
Compound wood pulp liquid is made of following procedure: mercerization wood pulp and softwood pulp 4:1 in mass ratio are mixed into obtain mixed serum,
Wood pulp concentration is 57wt%, and aluminum sulfate solution is added and aluminum stearate dissolution is uniformly mixed, the quality of aluminum sulfate is mixed serum
The 14wt% of quality, the pH value for adjusting slurries with sulfuric acid are then heated to 78 DEG C, are slowly added under 70r/min stirring condition to 4
Calcium hydroxide emulsion, the molar ratio of aluminum stearate, calcium hydroxide and aluminum sulfate are 0.2:1.8:1, then investment titanium esters acid is even rapidly
Join agent, nano hydrotalcite powder, the mass ratio of nano talc, titanium esters acid coupling agent and aluminum sulfate is 0.4:0.01:1, nanometer
The particle size range of hydrotalcite powder is 20~50nm, then proceedes to stirring 100min, stands to obtain compound wood pulp liquid；
Dipping solution is made of the following components: thermosetting phenolic resin 90g, PCTA copolymer 1 5g, crosslinking agent 4g, fire retardant 12g,
Styrene-acrylic emulsion 27g, methanol 250g, isopropyl acetate 25g, Organosilicon Alcohol in Organic sodium salt 4g；Fire retardant be Melamine Polyphosphate,
The compound of poly- methyltriethoxysilane and polyaluminium sulfate 2:2:1 in mass ratio composition.
The above-mentioned fire-retardant preparation method for solidifying filter paper, comprising the following steps:
(1) Ashless butyl diimide dispersant, defoaming agent, melamine tree are sequentially added under stirring condition into compound wood pulp liquid
Rouge and expanding material are uniformly mixed, and polyetherimide powder mixing is then added, adds polyethyleneimine and obtains paper pulp stoste；
(2) paper pulp stoste is beaten, beating degree is 37 ° of SR, and obtaining slurry concentration is 2.01% to be slurried, then in normal condition
Net is manufactured paper with pulp, press dewatering obtains body paper ontology, is heated to 175 DEG C of holding 80min, is subsequently placed in and is placed at room temperature for；
(3) thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and Organosilicon Alcohol in Organic sodium salt are placed in 75 in reaction kettle
It DEG C is uniformly mixed, is added after fire retardant mixes and adds crosslinking agent, PCTA copolymer is uniformly mixed and obtains maceration extract；
(4) the body paper ontology being placed at room temperature for obtained by step (2) is placed in maceration extract and is impregnated, sizing material is 17wt% in control, so
After be heated to 145 DEG C of solidification 7min, obtain fire-retardant solidification filter paper.
Embodiment 3
A kind of fire-retardant solidification filter paper, taking-up, which is heating and curing, after being impregnated in dipping solution by body paper ontology is made, in which:
Body paper ontology is made of the following components: compound wood pulp liquid 110g, polyetherimide powder 20g, polyethyleneimine 3g, trimerization
Melamine resin 3g, expanding material 5g, Ashless butyl diimide dispersant 6g, octanol 3g, expanding material are ethyl methacrylate and pyrrole
The pyridine mixture of 1:0.27 in mass ratio；
Compound wood pulp liquid is made of following procedure: mercerization wood pulp and softwood pulp 5:1 in mass ratio are mixed into obtain mixed serum,
Wood pulp concentration is 61.5wt%, and aluminum sulfate solution is added and aluminum stearate dissolution is uniformly mixed, the quality of aluminum sulfate is mixing slurry
The 16wt% of liquid quality, the pH value for adjusting slurries with sulfuric acid are then heated to 80 DEG C, slowly add under 80r/min stirring condition to 3
Enter calcium hydroxide emulsion, the molar ratio of aluminum stearate, calcium hydroxide and aluminum sulfate is 0.15:2:1, then investment titanium esters acid is even rapidly
Join agent, nano hydrotalcite powder, the mass ratio of nano talc, titanium esters acid coupling agent and aluminum sulfate is 0.5:0.02:1, nanometer
The particle size range of hydrotalcite powder is 20~50nm, then proceedes to stirring 120min, stands to obtain compound wood pulp liquid；
Dipping solution is made of the following components: thermosetting phenolic resin 100g, PCTA copolymer 20g, crosslinking agent 5g, fire retardant 15g,
Styrene-acrylic emulsion 30g, methanol 300g, isopropyl acetate 30g, Organosilicon Alcohol in Organic sodium salt 5g；Fire retardant be Melamine Polyphosphate,
The compound of poly- methyltriethoxysilane and polyaluminium sulfate 3:1:1 in mass ratio composition.
The above-mentioned fire-retardant preparation method for solidifying filter paper, comprising the following steps:
(1) Ashless butyl diimide dispersant, defoaming agent, melamine tree are sequentially added under stirring condition into compound wood pulp liquid
Rouge and expanding material are uniformly mixed, and polyetherimide powder mixing is then added, adds polyethyleneimine and obtains paper pulp stoste；
(2) paper pulp stoste is beaten, beating degree is 40 ° of SR, and obtaining slurry concentration is 2.11% to be slurried, then in normal condition
Net is manufactured paper with pulp, press dewatering obtains body paper ontology, is heated to 180 DEG C of holding 60min, is subsequently placed in and is placed at room temperature for；
(3) thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and Organosilicon Alcohol in Organic sodium salt are placed in 80 in reaction kettle
It DEG C is uniformly mixed, is added after fire retardant mixes and adds crosslinking agent, PCTA copolymer is uniformly mixed and obtains maceration extract；
(4) the body paper ontology being placed at room temperature for obtained by step (2) is placed in maceration extract and is impregnated, sizing material is 18wt% in control, so
After be heated to 150 DEG C of solidification 6min, obtain fire-retardant solidification filter paper.
Comparative example 1
It is prepared according to the method for embodiment 1 with raw material, difference from example 1 is that, the compound wood pulp liquid in raw material is
To polyaluminium sulfate is directly added in the mixed slurry of mercerization wood pulp and softwood pulp, additional amount is mixed serum quality
20wt%.
Comparative example 2
It is prepared according to the method for embodiment 1 with raw material, difference from example 1 is that, in the preparation process of body paper ontology
In, compound wood pulp liquid is beaten by the method for step (2) first, is then added in step (1) into the compound wood pulp liquid after mashing
Paper pulp stoste is obtained after raw material mixing in addition to compound wood pulp liquid, then manufactured paper with pulp, squeezed and obtain body paper ontology.
Comparative example 3
It is prepared according to the method for embodiment 1 with raw material, difference from example 1 is that, in the preparation process of body paper ontology,
Body paper ontology obtained by step (2) is directly impregnated in maceration extract when not heating and keeping, 150 DEG C is taken out and is heating and curing
8min。
Comparative example 4
It is prepared according to the method for embodiment 1 with raw material, difference from example 1 is that, in the configuration process of maceration extract,
Fire retardant used is the Melamine Polyphosphate of equivalent.
Comparative example 5
It is prepared according to the method for embodiment 1 with raw material, difference from example 1 is that, in the configuration process of maceration extract,
Fire retardant used is the Melamine Polyphosphate of equivalent and the mixture of poly- methyltriethoxysilane, and the two mass ratio is
2:1。
Solidify the performance indicators such as intensity, the air permeability of filter paper and referring to GB/ obtained by the various embodiments described above and comparative example
The results are shown in Table 1 for the flame retardant property index of T14656-2009 " fire retardant papers and cardboard combustibility test method " measurement,
When middle test bursting strength and stiffness, by it is to be tested solidify filter paper be first placed in 180 DEG C of baking oven keep the temperature 60min after re-test.
Claims (10)
1. a kind of fire-retardant solidification filter paper, which is characterized in that after the fire-retardant solidification filter paper is impregnated in dipping solution by body paper ontology
Taking-up, which is heating and curing, to be made, in which:
Body paper ontology is made of the component of following parts by weight: 100~120 parts of compound wood pulp liquid, polyetherimide powder 12~20
Part, 3~5 parts of polyethyleneimine, 2~4 parts of melamine resin, 2~5 parts of expanding material, Ashless butyl diimide dispersant 4~6
Part, 2~5 parts of defoaming agent；
Dipping solution is made of the component of following parts by weight: 80~100 parts of thermosetting phenolic resin, 0~20 part of PCTA copolymer 1,
2~5 parts of crosslinking agent, 8~15 parts of fire retardant, 25~30 parts of styrene-acrylic emulsion, 200~300 parts of methanol, isopropyl acetate 20~30
Part, 2~5 parts of Organosilicon Alcohol in Organic sodium salt.
2. fire-retardant solidification filter paper according to claim 1, which is characterized in that the compound wood pulp liquid is by following procedure system
At: mercerization wood pulp and softwood pulp 3~5:1 in mass ratio are mixed into obtain mixed serum, wood pulp concentration is 52.8~
61.5wt%, is added aluminum sulfate solution and aluminum stearate dissolution is uniformly mixed, and adjusts the pH value of slurries to 3~5, is then heated to
75~80 DEG C, calcium hydroxide emulsion is slowly added under 60~80r/min stirring condition, then rapidly investment titanium esters acid coupling agent, receive
Rice hydrotalcite powder, then proceedes to 90~120min of stirring, stands to obtain compound wood pulp liquid.
3. fire-retardant solidification filter paper according to claim 2, which is characterized in that the quality of the aluminum sulfate of addition is mixed serum
12~16wt% of quality, the molar ratio of aluminum stearate, calcium hydroxide and aluminum sulfate are 0.1~0.2:1.6~2:1, nano-talc
The mass ratio of powder, titanium esters acid coupling agent and aluminum sulfate is 0.3~0.5:0.01~0.02:1.
4. fire-retardant solidification filter paper according to claim 1 or 2, which is characterized in that the partial size of the nano hydrotalcite powder
Range is 20~50nm.
5. fire-retardant solidification filter paper according to claim 1 or 2, which is characterized in that the expanding material is methacrylic acid second
The mixture of ester and pyridine 1:0.2~0.3 in mass ratio.
6. fire-retardant solidification filter paper according to claim 1 or 2, which is characterized in that the defoaming agent is butanol or octanol.
7. fire-retardant solidification filter paper according to claim 1 or 2, which is characterized in that the fire retardant is melamine poly
The compound of phosphate, poly- methyltriethoxysilane and polyaluminium sulfate, the mass ratio of three are followed successively by 2~3:1~2:1.
8. the preparation method of the fire-retardant solidification filter paper as described in claim 1 to 7 is any, which comprises the following steps:
(1) Ashless butyl diimide dispersant, defoaming agent, melamine tree are sequentially added under stirring condition into compound wood pulp liquid
Rouge and expanding material are uniformly mixed, and polyetherimide powder mixing is then added, adds polyethyleneimine and obtains paper pulp stoste；
(2) paper pulp stoste is beaten, beating degree is 32~40 ° of SR, and obtaining slurry concentration is 1.82~2.11% to be slurried, then
Normal condition online is manufactured paper with pulp, press dewatering obtains body paper ontology, and then heating keeps being placed on being placed at room temperature for；
(3) thermosetting phenolic resin, methanol, isopropyl acetate, styrene-acrylic emulsion and Organosilicon Alcohol in Organic sodium salt are placed in 70 in reaction kettle
~80 DEG C are uniformly mixed, and are added after fire retardant mixes and add crosslinking agent, PCTA copolymer is uniformly mixed and obtains maceration extract；
(4) the body paper ontology that step (2) is placed at room temperature for is placed in maceration extract and is impregnated, sizing material is 17~18wt% in control, then
It is heating and curing, obtains fire-retardant solidification filter paper.
9. the fire-retardant preparation method for solidifying filter paper according to claim 8, which is characterized in that heating temperature in step (2)
It is 170~180 DEG C, 60~90min of retention time.
10. the fire-retardant preparation method for solidifying filter paper according to claim 8, which is characterized in that step (4) are heating and curing
Temperature is 140~150 DEG C, 6~8min of curing time.
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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 |