CN109880301A - A kind of New-type long-acting heat-resistant fireproof material and preparation method thereof - Google Patents
A kind of New-type long-acting heat-resistant fireproof material and preparation method thereof Download PDFInfo
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- CN109880301A CN109880301A CN201910224404.1A CN201910224404A CN109880301A CN 109880301 A CN109880301 A CN 109880301A CN 201910224404 A CN201910224404 A CN 201910224404A CN 109880301 A CN109880301 A CN 109880301A
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Landscapes
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- Tires In General (AREA)
Abstract
The invention discloses a kind of New-type long-acting heat-resistant fireproof materials and preparation method thereof, belong to technical field of polymer materials.The present invention mixes bamboo fibre with sodium hydroxide solution, stands, and filters, and washs, dry, obtains single treatment bamboo fibre；By single treatment bamboo fibre, Bacillus pasteurii bacterium solution, sucrose, urea, water mixed fermentation, then liquor alumini chloridi, ferric chloride solution and calcium nitrate solution add sodium hydroxide solution, adjust pH, mix, filter, dry, obtain secondary treatment bamboo fibre；Secondary treatment bamboo fibre is placed in retort, is heated up step by step, is carbonized, cooling obtains modified bamboo fiber；By epoxy resin, modified bamboo fiber, modified zeolite, organic siliconresin, odium stearate, cupric oxalate, silver oxalate, curing agent, phosphatide, essential oil mixing, injection molding, compression molding, demoulding is to get heat-resistant fireproof material.Heat-resistant fireproof material provided by the invention has excellent mechanical property and high temperature resistance and long-acting flame retardant property.
Description
Technical field
The invention discloses a kind of New-type long-acting heat-resistant fireproof materials and preparation method thereof, belong to high polymer material technology
Field.
Background technique
Fire retardant is classified by effective element, can be divided into phosphorus system, chlorine system, bromine system and antimony base, aluminium base, boryl fire retardant etc..It is existing
Product mainly has: the modified hydroxide of nanometric magnesium hydroxide fire retardant, high-purity industrial magnesium hydroxide fire retardant, high-purity technical grade
Magnesium fire retardant, magnesium hydroxide composite fire retardant, aluminium hydroxide fire retardant, modified aluminium hydroxide fire retardant, light magnesium oxide, insatiable hunger
With resin fire retardant, silicon rubber flame-retardant agent, polyamide fire retardant, PE fire retardant, PP fire retardant, PVC flame retardant, fire-retarding of wood
Agent, paper combustion inhibitor special, CPE fire retardant, fabric coating adhesive fire retardant, carpet back-adhesive fire retardant, water paint fire retardant, oil
Property apply material flame-retardant, powdery paints fire retardant, various ink fire retardants, the products such as heat stabilizer.Product is widely used to
ABS, CAB, PC, PS, natural rubber, butadiene-styrene rubber, neoprene, CSM, CPE, polyethylene, fluoropolymer, polyvinyl chloride,
Gather inclined two width ethylene, thermoplastic elastomer (TPE), silicon rubber, ethylene propylene diene rubber, nitrile rubber, PVC/ nitrile rubber blends,
In the rubber products such as EVA, blown rubber, PP, PA and engineering plastics product.The product of fire proofing can be divided mainly into fire-retardant knit
Object, fire retardant chemistry fiber, flame retardant plastics, flame retardant rubber, fireproof coating, fire-retardant wood-based materials and fire retardant papers, inorganic non-ignitable filling
7 major class such as material.Fire proofing be able to suppress or retardation burning and oneself be not easy to burning material, be widely used in
The fields such as clothes, petroleum, chemical industry, metallurgy, shipbuilding, fire-fighting, national defence.
It is related to the preparation difficult point of the fire proofing mainly balance between fire-retardant, high temperature resistant and toughness at present.Using having
Halogen fire retardant, material easily reach the fire-retardant V0 of 0.8-1.5mm.It is properly added the toughener of certain component, the stretching of material is strong
Degree will improve, but since toughener will affect Flame Retardancy, need to improve flame retardant compositions adding proportion in this way, and fire-retardant
Agent ratio increases, and can influence the toughness of material in turn, so, it at this moment just needs to adjust the proportion of the two components, makes
The anti-flammability and tensile strength of material reach best.
Summary of the invention
It is existing to solve the purpose of the present invention is to provide a kind of New-type long-acting heat-resistant fireproof material and preparation method thereof
The problems in technology.
To achieve the above object, the invention provides the following technical scheme:
A kind of New-type long-acting heat-resistant fireproof material, it is characterised in that: be made of the raw material of following parts by weight: 100~150
Part epoxy resin, 20~30 parts of bamboo fibres, 10~20 parts of zeolites, 2~3 parts of odium stearate, 10~20 parts of curing agent, 2~3 parts of phosphorus
Rouge, 2~3 parts of essential oils.
The heat-resistant fireproof material further includes the component of following parts by weight: 2~3 parts of cupric oxalates, 2~3 parts of silver oxalates,
10~20 parts of organic siliconresins.
The epoxy resin is any one in epoxy resin E51, epoxy resin E44 or epoxy resin E20；It is described solid
Agent is diethylenetriamine, any one in triethylene tetramine or dipropylenetriamine；The phosphatide is soybean lecithin or egg
Any one in yellow lecithin；The plants essential oil is Rosemary Oil, Lavender, rose ethereal oil, jasmine anthosin
Any one in oil, camellia essential oil or saussurea involucrata essential oil；The organic siliconresin is poly- methylsiloxane resin, and poly- ethyl is organic
Any one in silicone resin or poly- aryl organic siliconresin.
The heat-resistant fireproof material is made of the raw material of following parts by weight: 150 parts of epoxy resin, 30 parts of bamboo fibres
Dimension, 20 parts of zeolites, 3 parts of odium stearate, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts have
Machine silicone resin.
A kind of preparation method of New-type long-acting heat-resistant fireproof material, it is characterised in that: the heat-resistant fireproof material
Preparation method the following steps are included:
(1) bamboo fibre alkali soaks；
(2) step (1) gains are fermented, alkali process；
(3) step (2) gains are carbonized；
(4) it by zeolite pickling, ferments, charing；
(5) mixing, molding.
The preparation step of the heat-resistant fireproof material is as follows:
(1) bamboo fibre is mixed with sodium hydroxide solution, is stood, filtered, washed, it is dry, single treatment bamboo fibre is obtained, hydrogen is utilized
Sodium corrosion bamboo fibre is aoxidized, so that the permeance property of fiber gets a promotion；
(2) by single treatment bamboo fibre, Bacillus pasteurii bacterium solution, sucrose, urea, water mixed fermentation is subsequently added into aluminium chloride
Solution, ferric chloride solution and calcium nitrate solution add sodium hydroxide solution, adjust pH, are stirred, and filter, dry, obtain two
Secondary processing bamboo fibre, during the fermentation, Bacillus pasteurii generate urase in metabolic processes, and urase can will be in system
Urea decompose and generate carbanion and ammonium ion, since Bacillus pasteurii cell wall is negatively charged, in system
Calcium ion can be by Bacillus pasteurii Adsorption on cell walls, so that nano-calcium carbonate can be generated around bacterium using cell as nucleus
Calcium forms nanometer calcium carbonate microballoon, while utilizing the aluminium ion of the negatively charged enriched of Bacillus pasteurii cell wall
And iron ion, pH value then is adjusted by the way that sodium hydroxide solution is added dropwise, so that iron ion and aluminium ion precipitating in system, generate
Precipitating be dispersed in nanometer calcium carbonate microsphere surface, meanwhile, ammonium ion in system can be formed in conjunction with nitrate ion
Ammonium nitrate；
(3) secondary treatment bamboo fibre is carbonized, cools down, obtains modified bamboo fiber, the nanometer hydroxide in carbonization process, in system
Aluminium and nanometer ferric hydroxide precipitate dehydration generate nano aluminium oxide and nano iron oxide, meanwhile, heated point of the ammonium nitrate in fiber
Solution, generates gas, and the calcium carbonate microspheres in the gas diffusion carrying system of generation are distributed to fiber surface, on the one hand, gas
Rise motive force, so that calcium carbonate microspheres are entrenched in fiber surface, so that the flame retardance element in system not easily runs off, so that
The long-acting flame retardant property of product gets a promotion, meanwhile, calcium carbonate microspheres are entrenched in fiber surface, and the roughness of fiber surface is able to
It is promoted, so that mechanical snap is easily formed between fiber, so that the mechanical property of system is further promoted, another party
Face, since calcium carbonate microspheres are in hollow state, can effective trap heat so that the heat-proof quality of fiber gets a promotion, meanwhile,
The uphill process of calcium carbonate microspheres, so that a large amount of gap is left in fiber, so that the heat-proof quality of fiber obtains further
It is promoted, so that the high temperature resistance of system is further promoted；(4) by zeolite and hydrochloric acid 1:10~1 in mass ratio:
20 are stirred, and filter, and wash, dry, obtain pretreatment zeolite, according to parts by weight, by 20~30 parts of pretreatment zeolites, 8~
10 parts of cornstarch, 1~2 part of biogas slurry, 30~50 parts of water mixed fermentations are filtered, dry, are carbonized to get modified zeolite；
(5) by part epoxy resin, modified bamboo fiber, modified zeolite, organic siliconresin, odium stearate, cupric oxalate, silver oxalate, Gu
Agent, phosphatide, essential oil are stirred, injection molding, and compression molding demoulds to get heat-resistant fireproof material.
Specific preparation process is as follows for the heat-resistant fireproof material:
(1) sodium hydroxide solution 1:10~1:20 in mass ratio that bamboo fibre and mass fraction are 30~35% is placed in reaction kettle
In, after standing 5~8h, filtering obtains No. 1 filter cake, then with glacial acetic acid by No. 1 Washing of Filter Cake to neutrality, then by 1 after washing
Number filter cake is placed in baking oven, dry to constant weight under the conditions of temperature is 105~110 DEG C, obtains single treatment bamboo fibre；
(2) according to parts by weight, by 20~30 parts of single treatment bamboo fibres, 2~3 parts of Bacillus pasteurii bacterium solutions, 0.1~0.2
Part sucrose, 2~3 parts of urea, 30~50 parts of water are placed in No. 2 fermentation cauldrons, under the conditions of temperature is 28~32 DEG C, mixed fermentation 5
~8 days, the chlorine that 0.2~0.3 times of mass fraction of single treatment bamboo fibre quality is 10~20% is then added into No. 2 fermentation cauldrons
Change aluminum solutions, the ferric chloride solution and single treatment that 0.2~0.3 times of mass fraction of single treatment bamboo fibre quality is 10~20%
The calcium nitrate solution that 0.5~0.6 times of mass fraction of bamboo fibre quality is 10~20%, then mass fraction is added into fermentation cauldron and is
20~30% sodium hydroxide solution adjusts pH to 7.6~7.8, under the conditions of revolving speed is 300~500r/min, is stirred 40
After~60min, filtering obtains No. 2 filter cakes, then No. 2 filter cakes is placed in baking oven, under the conditions of temperature is 105~110 DEG C, does
It is dry to constant weight, obtain secondary treatment bamboo fibre；
(3) secondary treatment bamboo fibre is placed in retort, 60~90mL/min rate is filled with nitrogen into furnace, and with 8~10
DEG C/in-furnace temperature rises to 650~750 DEG C by min heating rate, and under the conditions of temperature is 650~750 DEG C, after carbonizing 2~3h,
It is down to room temperature with furnace, obtains modified bamboo fiber；
(4) hydrochloric acid 1:10~1:20 in mass ratio that zeolite and mass fraction are 20~30% is placed in No. 1 beaker, in revolving speed
Under the conditions of 500~600r/min, after being stirred 40~60min, filtering, obtain No. 1 filter residue, then with mass fraction be 20~
No. 1 residue washing to cleaning solution is neutrality by 30% ammonium hydroxide, and then No. 1 filter residue after washing is placed in baking oven, is in temperature
It is dry to constant weight under the conditions of 105~110 DEG C, pretreatment zeolite is obtained, according to parts by weight, and by 20~30 parts of pretreatment zeolites, 8
~10 parts of cornstarch, 1~2 part of biogas slurry, 30~50 parts of water are placed in No. 1 fermentation cauldron, under the conditions of temperature is 28~32 DEG C, are mixed
After closing fermentation 3~5 days, filtering obtains No. 2 filter residues, then No. 2 filter residues is placed in retort, and with 60~90mL/min rate
Think to be filled with argon gas in furnace, under the conditions of temperature is 700~800 DEG C, after carbonizing 2~3h, is down to room temperature with furnace and is boiled to get modified
Stone；
(5) according to parts by weight, by 100~150 parts of epoxy resin, 20~30 parts of modified bamboo fiber, 10~20 parts of modified zeolites,
10~20 parts of organic siliconresins, 2~3 parts of odium stearate, 2~3 parts of cupric oxalates, 2~3 parts of silver oxalates, 10~20 parts of curing agent, 2
~3 parts of phosphatide, 2~3 parts of essential oils are placed in batch mixer, under the conditions of revolving speed is 1100~1200r/min, it is stirred 40~
60min obtains mixed slurry, then by mixed slurry inject mold in, in temperature be 140~160 DEG C, pressure be 1.2~
Under the conditions of 1.8MPa, after compression molding, demould to get heat-resistant fireproof material.
Compared with prior art, the beneficial effects of the present invention are:
The present invention, which passes through, adds modified bamboo fiber, organic siliconresin, cupric oxalate, firstly, in the preparation process of modified bamboo fiber,
Corrode bamboo fibre using sodium hydroxide, so that the permeance property of fiber gets a promotion, so that it is logical so that its institutional framework is formed diffusion
Road is conducive in subsequent fermentations, and each component can penetrate sufficiently into inside institutional framework, then, during the fermentation,
Bacillus pasteurii generates urase in metabolic processes, urase the urea in system can be decomposed generate carbanion and
Ammonium ion, since Bacillus pasteurii cell wall is negatively charged, the calcium ion in system can be thin by Bacillus pasteurii
Cell wall absorption forms nanometer calcium carbonate microballoon, simultaneously to can generate nanometer calcium carbonate around bacterium using cell as nucleus
Since Bacillus pasteurii cell wall is negatively charged, so Bacillus pasteurii surface be capable of enriched aluminium ion and
Iron ion then adjusts pH value by the way that sodium hydroxide solution is added dropwise, so that iron ion and aluminium ion precipitating in system, generation
Precipitating is dispersed in nanometer calcium carbonate microsphere surface, meanwhile, the ammonium ion in system can form nitre in conjunction with nitrate ion
Sour ammonium, in carbonization process, nano-aluminum hydroxide and nanometer ferric hydroxide precipitate dehydration in system, generate nano aluminium oxide and
Nano iron oxide, meanwhile, the ammonium nitrate in fiber is thermally decomposed, and gas, the carbon in the gas diffusion carrying system of generation are generated
Sour calcium microballoon is distributed to fiber surface, on the one hand, the rising motive force of gas, so that calcium carbonate microspheres are entrenched in fiber surface,
So that the flame retardance element in system not easily runs off, so that the long-acting flame retardant property of product gets a promotion, meanwhile, calcium carbonate is micro-
Ball is entrenched in fiber surface, and the roughness of fiber surface is promoted, so that mechanical snap is easily formed between fiber, so that body
The mechanical property of system is further promoted, and on the other hand, since calcium carbonate microspheres are in hollow state, can effectively obstruct heat
Amount, so that the heat-proof quality of fiber gets a promotion, meanwhile, the uphill process of calcium carbonate microspheres, so that being left in fiber a large amount of
Gap, so that the heat-proof quality of fiber is further promoted, so that the high temperature resistance of system obtains further
It is promoted, secondly, the cupric oxalate in system is thermally decomposed under the conditions of high temperature fire, generates carbon dioxide, the carbon dioxide of generation
So that the modified bamboo fiber in system is further distributed into system surface, modified bamboo fiber is formed tightly on system surface
The close network of fibers entwined, meanwhile, when the temperature of system is more than the decomposition temperature of organic siliconresin, the silane of organic siliconresin
Key fracture is decomposed, and remaining silicon oxygen bond can be in conjunction with the nano aluminium oxide of fiber surface and nano iron oxide, in fiber table
Face forms silicon oxygen alloy layer, and silicon oxygen alloy layer has good heat-proof quality, so that system surface formation modified bamboo fiber is heat-insulated
Network, the effectively extraneous heat of barrier, so that the high temperature resistance of system is further promoted, meanwhile, silicon oxygen alloy
Layer can by system nano aluminium oxide and nano iron oxide be fixed in system, effectively prevent the stream of flame retardance element in system
It loses, so that the long-acting flame retardant property of product is further promoted.
Specific embodiment
Hydrochloric acid 1:10~1:20 in mass ratio that zeolite and mass fraction are 20~30% is placed in No. 1 beaker, in revolving speed
Under the conditions of 500~600r/min, after being stirred 40~60min, filtering, obtain No. 1 filter residue, then with mass fraction be 20~
No. 1 residue washing to cleaning solution is neutrality by 30% ammonium hydroxide, and then No. 1 filter residue after washing is placed in baking oven, is in temperature
It is dry to constant weight under the conditions of 105~110 DEG C, pretreatment zeolite is obtained, according to parts by weight, and by 20~30 parts of pretreatment zeolites, 8
~10 parts of cornstarch, 1~2 part of biogas slurry, 30~50 parts of water are placed in No. 1 fermentation cauldron, under the conditions of temperature is 28~32 DEG C, are mixed
After closing fermentation 3~5 days, filtering obtains No. 2 filter residues, then No. 2 filter residues is placed in retort, and with 60~90mL/min rate
Think to be filled with argon gas in furnace, under the conditions of temperature is 700~800 DEG C, after carbonizing 2~3h, is down to room temperature with furnace and is boiled to get modified
Stone；According to parts by weight, by 1~2 part of Bacillus pasteurii, 1~2 part of glycerol, 1~2 part of polyethylene glycol, 20~30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 32~35 DEG C in temperature, under the conditions of revolving speed is 200~300r/min, stirs
40~60min of mixing is mixed to get Bacillus pasteurii bacterium solution；Bamboo fibre is molten for 30~35% sodium hydroxide with mass fraction
Liquid 1:10~1:20 in mass ratio is placed in reaction kettle, and after standing 5~8h, filtering obtains No. 1 filter cake, then with glacial acetic acid by No. 1
No. 1 filter cake after washing is then placed in baking oven to neutrality, under the conditions of temperature is 105~110 DEG C, dries by Washing of Filter Cake
To constant weight, single treatment bamboo fibre is obtained；According to parts by weight, by 20~30 parts of single treatment bamboo fibres, 2~3 parts of Pasteur's gemma
Bacillus bacterium solution, 0.1~0.2 portion of sucrose, 2~3 parts of urea, 30~50 parts of water are placed in No. 2 fermentation cauldrons, in temperature be 28~32 DEG C
Under the conditions of, mixed fermentation 5~8 days, 0.2~0.3 times of quality of single treatment bamboo fibre quality point is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that number is 10~20%, the iron chloride that 0.2~0.3 times of mass fraction of single treatment bamboo fibre quality is 10~20%
The calcium nitrate solution that 0.5~0.6 times of mass fraction of solution and single treatment bamboo fibre quality is 10~20%, then into fermentation cauldron
Be added mass fraction be 20~30% sodium hydroxide solution, adjust pH to 7.6~7.8, in revolving speed be 300~500r/min item
Under part, after being stirred 40~60min, filtering, obtain No. 2 filter cakes, then No. 2 filter cakes be placed in baking oven, in temperature be 105~
It is dry to constant weight under the conditions of 110 DEG C, obtain secondary treatment bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 60~
90mL/min rate is filled with nitrogen into furnace, and in-furnace temperature is risen to 650~750 DEG C with 8~10 DEG C/min heating rate, in
Under the conditions of temperature is 650~750 DEG C, after carbonizing 2~3h, it is down to room temperature with furnace, obtains modified bamboo fiber；According to parts by weight, will
100~150 parts of epoxy resin, 20~30 parts of modified bamboo fiber, 10~20 parts of modified zeolites, 10~20 parts of organic siliconresins, 2~
3 parts of odium stearate, 2~3 parts of cupric oxalates, 2~3 parts of silver oxalates, 10~20 parts of curing agent, 2~3 parts of phosphatide, 2~3 parts of essential oils are set
In batch mixer, under the conditions of revolving speed is 1100~1200r/min, it is stirred 40~60min, obtains mixed slurry, then will
Mixed slurry injects in mold, is 140~160 DEG C in temperature, under the conditions of pressure is 1.2~1.8MPa, after compression molding, takes off
Mould is to get heat-resistant fireproof material.The epoxy resin is in epoxy resin E51, epoxy resin E44 or epoxy resin E20
Any one.The organic siliconresin is poly- methylsiloxane resin, poly- ethyl organic siliconresin or poly- aryl organic siliconresin
In any one.The curing agent is diethylenetriamine, any one in triethylene tetramine or dipropylenetriamine.The phosphorus
Rouge is any one in soybean lecithin or egg yolk lecithin.The plants essential oil is Rosemary Oil, Lavender, rose
Any one in rare flower essential oil, jasmine essential oil, camellia essential oil or saussurea involucrata essential oil.
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Example 1
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred
60min is to get Bacillus pasteurii bacterium solution；The sodium hydroxide solution 1:20 in mass ratio for being 35% by bamboo fibre and mass fraction
It is placed in reaction kettle, after standing 8h, filtering obtains No. 1 filter cake, then will then be washed No. 1 Washing of Filter Cake to neutrality with glacial acetic acid
No. 1 filter cake after washing is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains single treatment bamboo fibre；By weight
Number meter is measured, by 30 parts of single treatment bamboo fibres, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are set
In No. 2 fermentation cauldrons, under the conditions of temperature is 32 DEG C, mixed fermentation 8 days, single treatment bamboo is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that 0.3 times of mass fraction of fiber quality is 20%, 0.3 times of mass fraction of single treatment bamboo fibre quality are 20%
0.6 times of mass fraction of ferric chloride solution and single treatment bamboo fibre quality is 20% calcium nitrate solution, then is added into fermentation cauldron
The sodium hydroxide solution that mass fraction is 30% adjusts pH to 7.8, under the conditions of revolving speed is 500r/min, is stirred 60min
Afterwards, it filters, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain two
Secondary processing bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 90mL/min rate is filled with nitrogen into furnace, and with 10
DEG C/in-furnace temperature rises to 750 DEG C by min heating rate, under the conditions of temperature is 750 DEG C, after carbonizing 3h, it is down to room temperature with furnace,
Obtain modified bamboo fiber；According to parts by weight, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 20 parts have
Machine silicone resin, 3 parts of odium stearate, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils are placed in batch mixer
In, under the conditions of revolving speed is 1200r/min, it is stirred 60min, obtains mixed slurry, then injects mixed slurry in mold,
It is 160 DEG C in temperature, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.The epoxy
Resin is epoxy resin E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.Institute
Stating phosphatide is soybean lecithin.The plants essential oil is Rosemary Oil.
Example 2
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 150 parts of epoxy resin, 30 parts of nano aluminium oxides, 20 parts of modified zeolites, 20 parts
Organic siliconresin, 3 parts of odium stearate, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils are placed in mixing
In machine, under the conditions of revolving speed is 1200r/min, it is stirred 60min, mixed slurry is obtained, mixed slurry is then injected into mold
In, it is 160 DEG C in temperature, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.The ring
Oxygen resin is epoxy resin E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.
The phosphatide is soybean lecithin.The plants essential oil is Rosemary Oil.
Example 3
According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionized waters are placed in digital display survey
In fast constant temperature blender with magnetic force, it is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred 60min to get Pasteur's bud
Spore bacillus bacterium solution；The sodium hydroxide solution 1:20 in mass ratio that bamboo fibre and mass fraction are 35% is placed in reaction kettle, is stood
After 8h, filtering obtains No. 1 filter cake, then with glacial acetic acid by No. 1 Washing of Filter Cake to neutrality, is then placed in No. 1 filter cake after washing
It is dry to constant weight under the conditions of temperature is 110 DEG C in baking oven, obtain single treatment bamboo fibre；According to parts by weight, by 30 part one
Secondary processing bamboo fibre, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are placed in No. 2 fermentation cauldrons, Yu Wen
Under the conditions of degree is 32 DEG C, mixed fermentation 8 days, 0.3 times of quality of single treatment bamboo fibre quality point is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that number is 20%, the ferric chloride solution and primary place that 0.3 times of mass fraction of single treatment bamboo fibre quality is 20%
The calcium nitrate solution that 0.6 times of mass fraction of bamboo fibre quality is 20% is managed, then the hydrogen that mass fraction is 30% is added into fermentation cauldron
Sodium hydroxide solution adjusts pH to 7.8, and under the conditions of revolving speed is 500r/min, after being stirred 60min, filtering obtains No. 2 filter cakes,
Then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain secondary treatment bamboo fibre；By two
Secondary processing bamboo fibre is placed in retort, and 90mL/min rate is filled with nitrogen into furnace, and with 10 DEG C/min heating rate by furnace
Interior temperature rises to 750 DEG C, under the conditions of temperature is 750 DEG C, after carbonizing 3h, is down to room temperature with furnace, obtains modified bamboo fiber；By weight
Number meter, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 20 parts of organic siliconresins, 3 parts of stearic acid
Sodium, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils are placed in batch mixer, in revolving speed be 1200r/
Under the conditions of min, it is stirred 60min, obtains mixed slurry, then injects mixed slurry in mold, is 160 DEG C in temperature, presses
Under the conditions of power is 1.8MPa, after compression molding, demould to get heat-resistant fireproof material.The epoxy resin is epoxy resin
E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.The phosphatide is soybean ovum
Phosphatide.The plants essential oil is Rosemary Oil.
Example 4
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred
60min is to get Bacillus pasteurii bacterium solution；The sodium hydroxide solution 1:20 in mass ratio for being 35% by bamboo fibre and mass fraction
It is placed in reaction kettle, after standing 8h, filtering obtains No. 1 filter cake, then will then be washed No. 1 Washing of Filter Cake to neutrality with glacial acetic acid
No. 1 filter cake after washing is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains single treatment bamboo fibre；By weight
Number meter is measured, by 30 parts of single treatment bamboo fibres, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are set
In No. 2 fermentation cauldrons, under the conditions of temperature is 32 DEG C, mixed fermentation 8 days, single treatment bamboo is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that 0.3 times of mass fraction of fiber quality is 20%, 0.3 times of mass fraction of single treatment bamboo fibre quality are 20%
0.6 times of mass fraction of ferric chloride solution and single treatment bamboo fibre quality is 20% calcium nitrate solution, then is added into fermentation cauldron
The sodium hydroxide solution that mass fraction is 30% adjusts pH to 7.8, under the conditions of revolving speed is 500r/min, is stirred 60min
Afterwards, it filters, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain two
Secondary processing bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 90mL/min rate is filled with nitrogen into furnace, and with 10
DEG C/in-furnace temperature rises to 750 DEG C by min heating rate, under the conditions of temperature is 750 DEG C, after carbonizing 3h, it is down to room temperature with furnace,
Obtain modified bamboo fiber；According to parts by weight, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 3 parts of tristearin
Sour sodium, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils are placed in batch mixer, are in revolving speed
Under the conditions of 1200r/min, be stirred 60min, obtain mixed slurry, then by mixed slurry inject mold in, in temperature be 160
DEG C, under the conditions of pressure is 1.8MPa, after compression molding, demould to get heat-resistant fireproof material.The epoxy resin is asphalt mixtures modified by epoxy resin
Rouge E51.The curing agent is diethylenetriamine.The phosphatide is soybean lecithin.The plants essential oil is Rosemary Oil.
Example 5
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred
60min is to get Bacillus pasteurii bacterium solution；The sodium hydroxide solution 1:20 in mass ratio for being 35% by bamboo fibre and mass fraction
It is placed in reaction kettle, after standing 8h, filtering obtains No. 1 filter cake, then will then be washed No. 1 Washing of Filter Cake to neutrality with glacial acetic acid
No. 1 filter cake after washing is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains single treatment bamboo fibre；By weight
Number meter is measured, by 30 parts of single treatment bamboo fibres, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are set
In No. 2 fermentation cauldrons, under the conditions of temperature is 32 DEG C, mixed fermentation 8 days, single treatment bamboo is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that 0.3 times of mass fraction of fiber quality is 20%, 0.3 times of mass fraction of single treatment bamboo fibre quality are 20%
0.6 times of mass fraction of ferric chloride solution and single treatment bamboo fibre quality is 20% calcium nitrate solution, then is added into fermentation cauldron
The sodium hydroxide solution that mass fraction is 30% adjusts pH to 7.8, under the conditions of revolving speed is 500r/min, is stirred 60min
Afterwards, it filters, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain two
Secondary processing bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 90mL/min rate is filled with nitrogen into furnace, and with 10
DEG C/in-furnace temperature rises to 750 DEG C by min heating rate, under the conditions of temperature is 750 DEG C, after carbonizing 3h, it is down to room temperature with furnace,
Obtain modified bamboo fiber；According to parts by weight, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 20 parts have
Machine silicone resin, 3 parts of odium stearate, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils are placed in batch mixer, in revolving speed
Under the conditions of 1200r/min, it is stirred 60min, obtains mixed slurry, then mixed slurry is injected in mold, is in temperature
It 160 DEG C, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.The epoxy resin is ring
Oxygen resin E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.The phosphatide is
Soybean lecithin.The plants essential oil is Rosemary Oil.
Example 6
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred
60min is to get Bacillus pasteurii bacterium solution；The sodium hydroxide solution 1:20 in mass ratio for being 35% by bamboo fibre and mass fraction
It is placed in reaction kettle, after standing 8h, filtering obtains No. 1 filter cake, then will then be washed No. 1 Washing of Filter Cake to neutrality with glacial acetic acid
No. 1 filter cake after washing is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains single treatment bamboo fibre；By weight
Number meter is measured, by 30 parts of single treatment bamboo fibres, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are set
In No. 2 fermentation cauldrons, under the conditions of temperature is 32 DEG C, mixed fermentation 8 days, single treatment bamboo is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that 0.3 times of mass fraction of fiber quality is 20%, 0.3 times of mass fraction of single treatment bamboo fibre quality are 20%
0.6 times of mass fraction of ferric chloride solution and single treatment bamboo fibre quality is 20% calcium nitrate solution, then is added into fermentation cauldron
The sodium hydroxide solution that mass fraction is 30% adjusts pH to 7.8, under the conditions of revolving speed is 500r/min, is stirred 60min
Afterwards, it filters, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain two
Secondary processing bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 90mL/min rate is filled with nitrogen into furnace, and with 10
DEG C/in-furnace temperature rises to 750 DEG C by min heating rate, under the conditions of temperature is 750 DEG C, after carbonizing 3h, it is down to room temperature with furnace,
Obtain modified bamboo fiber；According to parts by weight, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 20 parts have
Machine silicone resin, 3 parts of odium stearate, 3 parts of cupric oxalates, 20 parts of curing agent, 3 parts of phosphatide, 3 parts of essential oils are placed in batch mixer, in revolving speed
Under the conditions of 1200r/min, it is stirred 60min, obtains mixed slurry, then mixed slurry is injected in mold, is in temperature
It 160 DEG C, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.The epoxy resin is ring
Oxygen resin E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.The phosphatide is
Soybean lecithin.The plants essential oil is Rosemary Oil.
Example 7
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred
60min is to get Bacillus pasteurii bacterium solution；The sodium hydroxide solution 1:20 in mass ratio for being 35% by bamboo fibre and mass fraction
It is placed in reaction kettle, after standing 8h, filtering obtains No. 1 filter cake, then will then be washed No. 1 Washing of Filter Cake to neutrality with glacial acetic acid
No. 1 filter cake after washing is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains single treatment bamboo fibre；By weight
Number meter is measured, by 30 parts of single treatment bamboo fibres, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are set
In No. 2 fermentation cauldrons, under the conditions of temperature is 32 DEG C, mixed fermentation 8 days, single treatment bamboo is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that 0.3 times of mass fraction of fiber quality is 20%, 0.3 times of mass fraction of single treatment bamboo fibre quality are 20%
0.6 times of mass fraction of ferric chloride solution and single treatment bamboo fibre quality is 20% calcium nitrate solution, then is added into fermentation cauldron
The sodium hydroxide solution that mass fraction is 30% adjusts pH to 7.8, under the conditions of revolving speed is 500r/min, is stirred 60min
Afterwards, it filters, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain two
Secondary processing bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 90mL/min rate is filled with nitrogen into furnace, and with 10
DEG C/in-furnace temperature rises to 750 DEG C by min heating rate, under the conditions of temperature is 750 DEG C, after carbonizing 3h, it is down to room temperature with furnace,
Obtain modified bamboo fiber；According to parts by weight, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 20 parts have
Machine silicone resin, 3 parts of odium stearate, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of essential oils are placed in batch mixer, in turn
Under the conditions of speed is 1200r/min, it is stirred 60min, obtains mixed slurry, then injected mixed slurry in mold, Yu Wendu
It is 160 DEG C, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.The epoxy resin is
Epoxy resin E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.The plant
Essential oil is Rosemary Oil.
Example 8
The hydrochloric acid 1:20 in mass ratio that zeolite and mass fraction are 30% is placed in No. 1 beaker, in revolving speed be 600r/min condition
Under, after being stirred 60min, filtering obtains No. 1 filter residue, and the ammonium hydroxide for being then 30% with mass fraction is by No. 1 residue washing to washing
Liquid is washed as neutrality, then No. 1 filter residue after washing is placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, it obtains
Zeolite is pre-processed, according to parts by weight, by 30 parts of pretreatment zeolites, 10 parts of cornstarch, 2 parts of biogas slurries, 50 parts of water are placed in No. 1 hair
In ferment kettle, under the conditions of temperature is 32 DEG C, after mixed fermentation 5 days, filtering obtains No. 2 filter residues, No. 2 filter residues is then placed in charing
In furnace, and think to be filled with argon gas in furnace with 90mL/min rate, under the conditions of temperature is 800 DEG C, after carbonizing 3h, is down to room with furnace
Temperature is to get modified zeolite；According to parts by weight, by 2 parts of Bacillus pasteuriis, 2 parts of glycerol, 2 parts of polyethylene glycol, 30 parts of deionizations
Water is placed in digital display and tests the speed in constant temperature blender with magnetic force, is 35 DEG C in temperature, under the conditions of revolving speed is 300r/min, is stirred
60min is to get Bacillus pasteurii bacterium solution；The sodium hydroxide solution 1:20 in mass ratio for being 35% by bamboo fibre and mass fraction
It is placed in reaction kettle, after standing 8h, filtering obtains No. 1 filter cake, then will then be washed No. 1 Washing of Filter Cake to neutrality with glacial acetic acid
No. 1 filter cake after washing is placed in baking oven, dry to constant weight under the conditions of temperature is 110 DEG C, obtains single treatment bamboo fibre；By weight
Number meter is measured, by 30 parts of single treatment bamboo fibres, 3 parts of Bacillus pasteurii bacterium solutions, 0.2 portion of sucrose, 3 parts of urea, 50 parts of water are set
In No. 2 fermentation cauldrons, under the conditions of temperature is 32 DEG C, mixed fermentation 8 days, single treatment bamboo is then added into No. 2 fermentation cauldrons
The liquor alumini chloridi that 0.3 times of mass fraction of fiber quality is 20%, 0.3 times of mass fraction of single treatment bamboo fibre quality are 20%
0.6 times of mass fraction of ferric chloride solution and single treatment bamboo fibre quality is 20% calcium nitrate solution, then is added into fermentation cauldron
The sodium hydroxide solution that mass fraction is 30% adjusts pH to 7.8, under the conditions of revolving speed is 500r/min, is stirred 60min
Afterwards, it filters, obtains No. 2 filter cakes, then No. 2 filter cakes are placed in baking oven, it is dry to constant weight under the conditions of temperature is 110 DEG C, obtain two
Secondary processing bamboo fibre；Secondary treatment bamboo fibre is placed in retort, 90mL/min rate is filled with nitrogen into furnace, and with 10
DEG C/in-furnace temperature rises to 750 DEG C by min heating rate, under the conditions of temperature is 750 DEG C, after carbonizing 3h, it is down to room temperature with furnace,
Obtain modified bamboo fiber；According to parts by weight, by 150 parts of epoxy resin, 30 parts of modified bamboo fiber, 20 parts of modified zeolites, 20 parts have
Machine silicone resin, 3 parts of odium stearate, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of curing agent, 3 parts of phosphatide are placed in batch mixer, in turn
Under the conditions of speed is 1200r/min, it is stirred 60min, obtains mixed slurry, then injected mixed slurry in mold, Yu Wendu
It is 160 DEG C, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.The epoxy resin is
Epoxy resin E51.The organic siliconresin is poly- methylsiloxane resin.The curing agent is diethylenetriamine.The phosphatide
For soybean lecithin.
Comparative example
According to parts by weight, by 150 parts of epoxy resin, 30 parts of nano aluminium oxides, 3 parts of odium stearate, 20 parts of curing agent are placed in mixed
In material machine, under the conditions of revolving speed is 1200r/min, it is stirred 60min, mixed slurry is obtained, mixed slurry is then injected into mould
In tool, it is 160 DEG C in temperature, under the conditions of pressure is 1.8MPa, after compression molding, demoulds to get heat-resistant fireproof material.It is described
Epoxy resin is epoxy resin E51.The curing agent is diethylenetriamine.
The resulting heat-resistant fireproof material of example 1 to 8 and comparative example product are subjected to performance detection, specific detection method is such as
Under:
1. mechanical property: detecting test specimen tensile strength referring to GB/T528；
2. long-acting flame retardant property: detecting test specimen oxygen index (OI) according to GB/T10707, after 3 months, detect its limit oxygen index again；
3. high temperature resistance: DHX-9143 type electric heating constant temperature air blast ageing oven (Shanghai Fuma Experiment Equipment Co., Ltd.) is used,
Experiment condition: aging temperature: 200 DEG C, the time: 48 hours.
Mechanical property and the specific testing result of long-acting flame retardant property are as shown in table 1:
Table 1:
The specific testing result of high temperature resistance is as shown in table 2:
After thermo-oxidative ageing (in air, 200 ± 1 DEG C, 48h)
By Tables 1 and 2 testing result it is found that by example 1, example 2 and comparative example are compared, and the present invention is fine by addition modified bamboo
Dimension, modified bamboo fiber are prepared by a series of means, so that a large amount of raised microballoon is contained on its surface, in use process
In, Yi Fasheng mechanical snap, so that the mechanical property of system gets a promotion, simultaneously as the protrusion on modified bamboo fiber surface is
Hollow calcium carbonate microspheres, and due to the impetus of gas, so that fibrous inside is hollow, and by example 1, example 5 and comparison
Example comparison, under the conditions of high temperature fire, the cupric oxalate in system is thermally decomposed, and generates carbon dioxide, and the carbon dioxide of generation makes
Modified bamboo fiber in system is further distributed into system surface, the webbed fibrous insulating layer of shape so that heat be difficult into
Enter system, so that system is not easy to reach ignition point, so that the flame retardant property of system gets a promotion, meanwhile, so that inside system
Resin is difficult to reach softening point, so that the high temperature stability performance of product gets a promotion；
By Tables 1 and 2 testing result it is found that by example 1, example 4 and comparative example are compared, and the present invention is by utilizing organosilicon tree
Rouge, under the conditions of high temperature fire, organic siliconresin is decomposed, the nano particle knot of free radical and modified bamboo fiber surface after decomposition
It closes, on the one hand, forming conjugate effectively can prevent heat from entering system, so that the high temperature stability performance of system gets a promotion,
On the other hand, so that the fire-retardant particle in system is effectively fixed, the loss of flame retardance element is effectively prevented, so that product
Long-acting flame retardant property gets a promotion, so heat-resistant fireproof material provided by the invention has excellent fire-retardant, high temperature resistant and power
Performance is learned, is had a wide range of applications in fire proofing field.
It is obvious to a person skilled in the art that invention is not limited to the details of the above exemplary embodiments, Er Qie
In the case where without departing substantially from spirit or essential attributes of the invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, the present embodiments are to be considered as illustrative and not restrictive, and the scope of the present invention is by appended power
Benefit requires rather than above description limits, it is intended that all by what is fallen within the meaning and scope of the equivalent elements of the claims
Variation is included within the present invention, and should not be construed as limiting the claims involved any label in claim.
Claims (7)
1. a kind of New-type long-acting heat-resistant fireproof material, it is characterised in that: be made of the raw material of following parts by weight: 100~
150 parts of epoxy resin, 20~30 parts of bamboo fibres, 10~20 parts of zeolites, 2~3 parts of odium stearate, 10~20 parts of curing agent, 2~3
Part phosphatide, 2~3 parts of essential oils.
2. a kind of New-type long-acting heat-resistant fireproof material according to claim 1, it is characterised in that: the heat-resistant fireproof
Material further includes the component of following parts by weight: 2~3 parts of cupric oxalates, 2~3 parts of silver oxalates, 10~20 parts of organic siliconresins.
3. a kind of New-type long-acting heat-resistant fireproof material according to claim 2, it is characterised in that: the epoxy resin is ring
Any one in oxygen resin E51, epoxy resin E44 or epoxy resin E20；The curing agent is diethylenetriamine, triethylene
Any one in tetramine or dipropylenetriamine；The phosphatide is any one in soybean lecithin or egg yolk lecithin；Institute
Stating plants essential oil is Rosemary Oil, Lavender, rose ethereal oil, jasmine essential oil, in camellia essential oil or saussurea involucrata essential oil
Any one；The organic siliconresin is poly- methylsiloxane resin, poly- ethyl organic siliconresin or poly- aryl organosilicon tree
Any one in rouge.
4. a kind of New-type long-acting heat-resistant fireproof material according to claim 3, it is characterised in that: the heat-resistant fireproof material
Material is made of the raw material of following parts by weight: 150 parts of epoxy resin, 30 parts of bamboo fibres, 20 parts of zeolites, 3 parts of odium stearate, and 20
Part curing agent, 3 parts of phosphatide, 3 parts of essential oils, 3 parts of cupric oxalates, 3 parts of silver oxalates, 20 parts of organic siliconresins.
5. a kind of preparation method of New-type long-acting heat-resistant fireproof material, it is characterised in that: the system of the heat-resistant fireproof material
Preparation Method the following steps are included:
The leaching of bamboo fibre alkali；
Step (1) gains are fermented, alkali process；
Step (2) gains are carbonized；
By zeolite pickling, ferment, charing；
Mixing, molding.
6. a kind of preparation method of New-type long-acting heat-resistant fireproof material according to claim 5, it is characterised in that: described resistance to
The preparation step of high temperature flame-proof material is as follows:
(1) bamboo fibre is mixed with sodium hydroxide solution, is stood, filtered, washed, it is dry, obtain single treatment bamboo fibre；
(2) by single treatment bamboo fibre, Bacillus pasteurii bacterium solution, sucrose, urea, water mixed fermentation is subsequently added into aluminium chloride
Solution, ferric chloride solution and calcium nitrate solution add sodium hydroxide solution, adjust pH, are stirred, and filter, dry, obtain two
Secondary processing bamboo fibre；
(3) it by secondary treatment bamboo fibre, carbonizes, cooling obtains modified bamboo fiber；
(4) zeolite and hydrochloric acid are stirred, are filtered, washed, it is dry, pretreatment zeolite is obtained, zeolite will be pre-processed, corn forms sediment
Powder, biogas slurry, water mixed fermentation are filtered, dry, are carbonized to get modified zeolite；
(5) by part epoxy resin, modified bamboo fiber, modified zeolite, organic siliconresin, odium stearate, cupric oxalate, silver oxalate, Gu
Agent, phosphatide, essential oil are stirred, injection molding, and compression molding demoulds to get heat-resistant fireproof material.
7. a kind of preparation method of New-type long-acting heat-resistant fireproof material according to claim 6, it is characterised in that: described resistance to
Specific preparation process is as follows for high temperature flame-proof material:
Sodium hydroxide solution 1:10~1:20 in mass ratio that bamboo fibre and mass fraction are 30~35% is placed in reaction kettle,
After standing 5~8h, filtering obtains No. 1 filter cake, then with glacial acetic acid by No. 1 Washing of Filter Cake to neutrality, then by No. 1 after washing
Filter cake is placed in baking oven, dry to constant weight under the conditions of temperature is 105~110 DEG C, obtains single treatment bamboo fibre；
According to parts by weight, by 20~30 parts of single treatment bamboo fibres, 2~3 parts of Bacillus pasteurii bacterium solutions, 0.1~0.2 part of sugarcane
Sugar, 2~3 parts of urea, 30~50 parts of water are placed in No. 2 fermentation cauldrons, under the conditions of temperature is 28~32 DEG C, mixed fermentation 5~8
It, is then added the aluminium chloride that 0.2~0.3 times of mass fraction of single treatment bamboo fibre quality is 10~20% into No. 2 fermentation cauldrons
Solution, the ferric chloride solution and single treatment bamboo that 0.2~0.3 times of mass fraction of single treatment bamboo fibre quality is 10~20% are fine
Tie up 0.5~0.6 times of mass fraction of quality be 10~20% calcium nitrate solution, then into fermentation cauldron be added mass fraction be 20~
30% sodium hydroxide solution adjusts pH to 7.6~7.8, under the conditions of revolving speed is 300~500r/min, it is stirred 40~
After 60min, filtering obtains No. 2 filter cakes, then No. 2 filter cakes is placed in baking oven, dry under the conditions of temperature is 105~110 DEG C
To constant weight, secondary treatment bamboo fibre is obtained；
Secondary treatment bamboo fibre is placed in retort, 60~90mL/min rate is filled with nitrogen into furnace, and with 8~10 DEG C/
In-furnace temperature is risen to 650~750 DEG C by min heating rate, under the conditions of temperature is 650~750 DEG C, after carbonizing 2~3h, with furnace
It is down to room temperature, obtains modified bamboo fiber；
Hydrochloric acid 1:10~1:20 in mass ratio that zeolite and mass fraction are 20~30% is placed in No. 1 beaker, is in revolving speed
Under the conditions of 500~600r/min, after being stirred 40~60min, filtering, obtain No. 1 filter residue, then with mass fraction be 20~
No. 1 residue washing to cleaning solution is neutrality by 30% ammonium hydroxide, and then No. 1 filter residue after washing is placed in baking oven, is in temperature
It is dry to constant weight under the conditions of 105~110 DEG C, pretreatment zeolite is obtained, according to parts by weight, and by 20~30 parts of pretreatment zeolites, 8
~10 parts of cornstarch, 1~2 part of biogas slurry, 30~50 parts of water are placed in No. 1 fermentation cauldron, under the conditions of temperature is 28~32 DEG C, are mixed
After closing fermentation 3~5 days, filtering obtains No. 2 filter residues, then No. 2 filter residues is placed in retort, and with 60~90mL/min rate
Think to be filled with argon gas in furnace, under the conditions of temperature is 700~800 DEG C, after carbonizing 2~3h, is down to room temperature with furnace and is boiled to get modified
Stone；
According to parts by weight, by 100~150 parts of epoxy resin, 20~30 parts of modified bamboo fiber, 10~20 parts of modified zeolites, 10
~20 parts of organic siliconresins, 2~3 parts of odium stearate, 2~3 parts of cupric oxalates, 2~3 parts of silver oxalates, 10~20 parts of curing agent, 2~3
Part phosphatide, 2~3 parts of essential oils are placed in batch mixer, under the conditions of revolving speed is 1100~1200r/min, it is stirred 40~
60min obtains mixed slurry, then by mixed slurry inject mold in, in temperature be 140~160 DEG C, pressure be 1.2~
Under the conditions of 1.8MPa, after compression molding, demould to get heat-resistant fireproof material.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113828311A (en) * | 2021-10-14 | 2021-12-24 | 西安建筑科技大学 | High-sulfur-resistance catalyst for removing CO and preparation method thereof |
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| CN109233207A (en) * | 2018-09-20 | 2019-01-18 | 贵州西南制造产业园有限公司 | A kind of insulating materials and preparation method thereof for cable connector |
| CN109280337A (en) * | 2018-09-17 | 2019-01-29 | 佛山皖和新能源科技有限公司 | A kind of preparation method of refractory glass fibre insulation board |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109280337A (en) * | 2018-09-17 | 2019-01-29 | 佛山皖和新能源科技有限公司 | A kind of preparation method of refractory glass fibre insulation board |
| CN109233207A (en) * | 2018-09-20 | 2019-01-18 | 贵州西南制造产业园有限公司 | A kind of insulating materials and preparation method thereof for cable connector |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113828311A (en) * | 2021-10-14 | 2021-12-24 | 西安建筑科技大学 | High-sulfur-resistance catalyst for removing CO and preparation method thereof |
| CN113828311B (en) * | 2021-10-14 | 2024-03-22 | 西安建筑科技大学 | High sulfur-resistant catalyst for removing CO and preparation method thereof |
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