CN109278151A - A kind of preparation method of fire protection flame retarding denseness sheet material - Google Patents
A kind of preparation method of fire protection flame retarding denseness sheet material Download PDFInfo
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- CN109278151A CN109278151A CN201811208169.0A CN201811208169A CN109278151A CN 109278151 A CN109278151 A CN 109278151A CN 201811208169 A CN201811208169 A CN 201811208169A CN 109278151 A CN109278151 A CN 109278151A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/10—Moulding of mats
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
- B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
- B27K3/10—Apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/18—Auxiliary operations, e.g. preheating, humidifying, cutting-off
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27N—MANUFACTURE BY DRY PROCESSES OF ARTICLES, WITH OR WITHOUT ORGANIC BINDING AGENTS, MADE FROM PARTICLES OR FIBRES CONSISTING OF WOOD OR OTHER LIGNOCELLULOSIC OR LIKE ORGANIC MATERIAL
- B27N3/00—Manufacture of substantially flat articles, e.g. boards, from particles or fibres
- B27N3/08—Moulding or pressing
- B27N3/18—Auxiliary operations, e.g. preheating, humidifying, cutting-off
- B27N3/183—Forming the mat-edges, e.g. by cutting
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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Forests & Forestry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The present invention relates to plate manufacturing technology fields, more particularly to a kind of preparation method of fire protection flame retarding denseness sheet material, it is included in and prepares base fiber, prepare reinforcing fiber, prepare binder, prepare fire-retardant enhancers, prepare curing agent, material mixing and plate preparation.Plate preparation method of the invention, waste is reused, it is environmentally protective, the plate mechanical strength of preparation is preferable, has excellent mildew-proof flame retarded performance, no pernicious gas release, production process is controllable, it is nontoxic, suitable for mass production, practical value with higher and good application prospect.
Description
Technical field
The present invention relates to modern paper technical fields, and in particular to a kind of preparation method of fire protection flame retarding denseness sheet material.
Background technique
On the one hand, timber is constantly subjected to the favor of the mankind, natural texture, texture, structural mechanical property, workability
Etc. being that other materials can not be substituted, it is used widely in furniture manufacturing industry and building material industry.However part timber, especially
The material of artificial forest wood is not able to satisfy public needs, such as its structure is of a relatively loose, density is low, is easily damaged by insects, bacterium erosion, acid,
Alkali and weathering degradation etc., therefore composite board is applied and is given birth to, and existing plate chinese raw materials is excessively single, the plate prepared is resistance to
Pressure and mechanical performance are bad.
Another aspect fire-retarding of wood is the method for improving timber fire-resistant ability with physical method or chemical method, it is therefore an objective to be hindered
Slow combustion of wood, with the generation of fire preventing, or quickly eliminates the fire occurred.Common wood fire retardant presses contained element
Composition can be divided mainly into: halogen flame, phosphorus-nitrogenated flame retardant, boron flame retardant and metal hydroxide combustion inhibitor etc..Its
In, it is most commonly that aluminium hydroxide and magnesium hydroxide in metal hydroxide combustion inhibitor, is released at high temperature due to them
A large amount of water vapours can dilute combustible concentration, thus can delay the thermal degradation speed of material, slow down or inhibit the burning of material,
And promote to carbonize and press down cigarette.In addition, itself is nontoxic, non-volatile for metal hydroxide combustion inhibitor, burning does not generate toxic and rotten
Corrosion gas is at home and abroad known as nuisanceless fire retardant.But common aluminium hydroxide, magnesium hydroxide but in the prevalence of
The low problem of flame retarding efficiency.
Furthermore existing anticorrosive wood is to pass through common wood after artificial addition chemical preservative, makes it have anti-corrosion
The characteristics such as erosion, moisture-proof, anti-fungal, ant prevention, anti-mildew and waterproof.Soil and wet environment can be directly contacted, is often made
Used in outdoor flooring, engineering, landscape, it is outdoor flooring, gardens that wild beauty is had a rest for people and appreciated to anticorrosive wood flower stand etc.
The ideal material of landscape, the wooden swing, recreational facilities, wooden footway etc., and existing preservative mould inhibitor anti-mold effect is not strong, application
It can not effectively achieve the desired results, need to improve in plate.
Summary of the invention
In view of the drawbacks of the prior art, the object of the present invention is to provide a kind of preparation method of fire protection flame retarding denseness sheet material,
Waste can be reused, environmentally protective, the plate mechanical strength of preparation is preferable, with excellent mildew-proof flame retarded
Performance, the release of no pernicious gas, production process is controllable, nontoxic, suitable for mass production, practical value with higher and good
Good application prospect.
The present invention solves technical problem and adopts the following technical scheme that
The present invention provides a kind of preparation methods of fire protection flame retarding denseness sheet material, comprising the following steps:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
5-7h is kept the temperature at being 50-70 DEG C in temperature in addition steamer, then carries out pressure cooking 1-2h, is then ground, is sent using defibrator
Enter closed pressure vessel, kept for 10 minutes under 2Mpa air pressure, mixed material is filtered after moment opening closed container, to mixture
Material carries out rolling rubbing, be added after drying butyl titanate 4-6 parts by weight, 40-50 parts of dehydrated alcohol, mass fraction be
In the dipping solution that 35% 10-15 parts of Adlerika, 15-20 parts of polyvinyl alcohol proportions are formed, stirring is impregnated 20-30 minutes, drip
It does spare；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
24-48h is impregnated in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, then is washed with water,
It is sent into high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done standby
With；
Step 3 adds 2-4 parts of dimethylolpropionic acid and 17-19 parts of methyl diphenylene diisocyanate mixing according to parts by weight
Enter in 20-30 parts of acetone soln, is reacted 80-120 minutes at 45-55 DEG C, add 7-9 parts of modification of chitosan at room temperature
Magnetic agitation 5min-10min, mixing speed be 200-300r/min, add 5-6 parts after coupling agent modified magnalium receive
Rice layered double hydroxide, 3-5 parts of melamines, 0.1-0.2 parts of metal quantum points and the double phenoxazine arsenic of 0.5-1 parts of oxos exist
10-20 minutes under high-speed stirred, ultrasonic treatment is carried out 30-50 minutes at being 70-80 DEG C in temperature, cooling is spare；
It is described it is coupling agent modified after magnalium nano-layered double hydroxides the preparation method comprises the following steps:
3:1 weighs Al (NO in molar ratio3)3·9H2O and Mg (NO3)2·6H2O is dissolved in distilled water, is stirred evenly, at 4-6 DEG C
It is lower quickly to instill lye, it adjusts pH and is reacted within the scope of 9.4-9.6 30-40 minutes, disperse distillation for filter cake after filtering washing
In water, it is cooled to room temperature to obtain transparent whites slurry after 18 h are reacted at 120 DEG C, centrifugal drying grinds the product after drying
Carefully to 30-40 μm, then the coupling agent of mass percent concentration 15-25% is hydrolyzed 20-30 minutes at room temperature, in ultrasonic wave
It is added with stirring finely ground rear product, at 80-90 DEG C, after filtering, wash after reaction 1-2h, being dry to obtain the final product；
Step 4: by weight crushing 7-9 parts of energy stones for partial size is 200 mesh particles, it is added in 5-7 parts of acetone and is heated to
It 60 DEG C, adds 20-60 parts of polyethylene glycol 1500s, 15-35 portions of mannitol, shear dispersion under 2500-3500r/min revolving speed
10-20min；Then 8-10 parts of algae clay, 5-9 parts of expanded graphite, 1-3 are sequentially added under 100-200 r/min revolving speed
The active carbon of part, which is added in dispersion machine, to be dispersed, and 10-14 parts of ammonium polyphosphate, 1-3 parts are sequentially added under 100-200 r/min revolving speed
Pentaerythrite, 1-2 parts of potassium peroxydisulfates and 0.5-0.9 parts of ferric sulfate continue the shearing dispersion 15- under 3500-4500r/min revolving speed
30min, then be transferred in sand mill and be sanded to 1 μm of fineness <, it is spare；
Step 5: by weight by 25-35 parts of lauryl methacrylates, 10-20 parts of 13 carbon esters of methacrylic acid, 15-25
Part acrylamide, 5-10 parts of ethyoxyl sodium alkyl sulfates and 2-4 parts of APES formaldehyde condensation products are stirred in advance,
0 .3-0.5 parts of ammonium sulfate is added into the pre- agitating solution again, 3-6h is then reacted at 73-76 DEG C, it is spare；
Step 6: the mixture prepared 80-90 parts of step 1 according to parts by weight and three mixtures prepared the step of 4-10 parts
It is added in high speed mixer, is mixed 2-4 minutes, the mixture for adding the preparation of 40-50 parts of step 2 continues to stir, then will
The material for puddling end is sent into vacuum roll mill, is 60-70 DEG C in temperature, and humidity is at roll-in 10-20 points repeatedly of 25%-35%
It is spare to obtain pretreatment material for clock；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 10-20min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure leaching
In stain agitator tank, 0.7-1.5MPa pressure is added to stir 30-50 minutes；Draining valve and the complete pressure release of gas valve are successively opened,
Then it is again turned on vacuum pump to vacuumize, keeps pressure inside the tank to be 0 .01-0 .02MPa and maintain 10-20min, take out mixing
Object；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains plate within precompressed 5-7 minutes in the case where pressure is 1.5-2.0Mpa, temperature is 85-95 DEG C
Material parison, by the mixture prepared in step 5 be coated in plate preform surface, control glue spreader temperature be 140-160 DEG C,
Coated weight is 100-150g/m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge i.e.
?.
Preferably, the metal quantum point in the step 3 is prepared using following methods:
It by weight disperses the titanium dioxide of 3-5 parts of 100nm-200nm in 40-50 parts of alcohol solution, is added 1-2 parts
Silver nitrate, 4-6 a part ethylenediamine pass sequentially through in hydrothermal reaction kettle, are kept for 10-14 hours in 140-180 DEG C, are down to room temperature mistake
It filters to obtain the final product.
Preferably, the multiple molding in the step 8 specifically:
Will treated plate parison in moulding press, be first that the 150-160 DEG C of pressure with 10-12Mpa suppresses 40- in temperature
60s is cooled to the 130-140 DEG C of pressure with 6-8Mpa and suppresses 80-120s, then is cooled to the 110-120 DEG C of pressure with 2-4Mpa
Suppress 180-240s.
Preferably, the modification of chitosan is the NH on epoxychloropropane and chitosan2Reaction is modified with ethylenediamine makes again
The ethylenediamine modified crosslinking chitosan magnetic obtained and thiourea modified, glutaraldehyde cross-linking the magnetism prepared with inverse suspension crosslinking method
The mixture that chitosan is formed according to weight ratio 3:2.
Preferably, it is described increase property plant extracts the preparation method comprises the following steps: by Dalmatian chrysanthemum, Folium Forsythia, camphortree leaf, crane grass according to
After weight ratio 2:3:1:1 is crushed plus water pretreatment is made using multiple counter-current extraction, shove and vacuum concentration, wherein extract
Time is 60min, amount of water is plant weight 6 times, degree of extracting be 40%, extraction times are 6 times, temperature concentrated in vacuo 45
±2℃。
Preferably, the expanded graphite the preparation method comprises the following steps:
According to mass ratio 1:1.2:0.2:1.5, by crystalline flake graphite, nitric acid, hydrogen peroxide and phosphoric acid, temperature is that 80 points are reacted at 40 DEG C again
Clock, then the sulphur-free expanded graphite that swelling volume is 312ml/g is prepared at being 900 DEG C in swelling temperature.
Preferably, the step 3 are as follows:
20-30 is added in the 17-19 parts of mixing of 2-4 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate according to parts by weight
Part acetone soln in, reacted 80-120 minutes at 45-55 DEG C, adding 7-9 parts of modification of chitosan, magnetic force stirs at room temperature
5min-10min is mixed, mixing speed is 200-300r/min, adds the 5-6 parts of magnalium nano lamellars after coupling agent modified
The double phenoxazine arsenic of double-metal hydroxide, 3-5 part melamine, 0.1-0.2 parts of metal quantum points, 0.5-1 parts of oxos and 3-5 parts
C9 Petropols 10-20 minutes under high velocity agitation, ultrasonic treatment is carried out 30-50 minutes at being 70-80 DEG C in temperature, cooling is standby
With.
Preferably, the step 6 are as follows:
The mixture that is prepared according to parts by weight by the step of mixture prepared by 80-90 parts of step 1,7-15 parts three, 2-4 parts
Borax and 1-2 parts of zinc borate are added in high speed mixer, are mixed 2-4 minutes, add 40-50 parts of step 2 preparations
Mixture continues to stir, then the material for puddling end is sent into vacuum roll mill, is 60-70 DEG C in temperature, humidity is in 25%-
35% roll-in 10-20 minutes repeatedly, it is spare to obtain pretreatment material.
Preferably, fire protection flame retarding denseness sheet material preparation method the following steps are included:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
6h is kept the temperature at being 60 DEG C in temperature in addition steamer, then carries out pressure cooking 1.5h, is then ground using defibrator, feeding is closed
Pressure vessel is kept for 10 minutes under 2Mpa air pressure, is filtered mixed material after moment opening closed container, is carried out to mixed material
Rubbing is rolled, it is 35% Adlerika that 5 parts of butyl titanate, 45 parts of dehydrated alcohol, mass fraction by weight are added after drying
In the dipping solution of 12 parts, 18 parts of polyvinyl alcohol proportion formation, stirring is impregnated 25 minutes, drained and standby；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
36h is impregnated in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, then is washed with water, is sent
Enter high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done spare；
The 18 parts of mixing of 2-4 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate are added according to parts by weight for step 3
It in 25 parts of acetone soln, is reacted 100 minutes at 50 DEG C, adds 8 parts of modification of chitosan magnetic agitation 7min at room temperature,
Mixing speed is 250r/min, adds 5.5 parts of magnalium nano-layered double hydroxides after coupling agent modified, 4 parts
Melamine, 0.15 part of metal quantum point and 0.7 part of oxo double phenoxazine arsenic 15 minutes under high velocity agitation, in the case where temperature is 75 DEG C
Carry out ultrasonic treatment 40 minutes, cooling is spare；
Step 4: by weight crushing the energy stone that 8 parts of partial sizes are 2cm for partial size is 200 mesh particles, 6 parts of acetone is added
In be heated to 60 DEG C, add 40 parts of polyethylene glycol 1500s, 25 portions of mannitol, under 3000r/min revolving speed shear dispersion
15min；Then 9 parts of algae clay, 7 parts of expanded graphite, 2 parts of active carbon are sequentially added under 150r/min revolving speed and is added divides
Dissipate and disperse in machine, sequentially add 12 parts of ammonium polyphosphate, 2 parts of pentaerythrites under 150r/min revolving speed, 1.5 parts of potassium peroxydisulfates and
0.7 part of ferric sulfate continues the shearing dispersion 19min under 4000r/min revolving speed, then is transferred in sand mill and is sanded to 1 μm of fineness <,
It is spare；
Step 5: by weight by 30 parts of lauryl methacrylates, 15 parts of 13 carbon esters of methacrylic acid, 20 parts of acryloyls
Amine, 7 parts of ethyoxyl sodium alkyl sulfates and 3 parts of APES formaldehyde condensation products are stirred in advance, then pre- are stirred to described
0.4 part of ammonium sulfate of addition in solution is mixed, 4.5h is then reacted at 75 DEG C, it is spare；
Step 6: the mixtures that the step of mixture prepared by 85 parts of step 1 and 7 parts three prepare are added according to parts by weight high
It in fast batch mixer, is mixed 3 minutes, the mixture for adding the preparation of 45 parts of step 2 continues to stir, then will puddle end
Material is sent into vacuum roll mill, is 65 DEG C in temperature, and it is spare to obtain pretreatment material in 30% roll-in 15 minutes repeatedly for humidity；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 15min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure impregnation
In agitator tank, 1.1MPa pressure is added to stir 40 minutes；Draining valve and the complete pressure release of gas valve are successively opened, is then opened again
It opens vacuum pump to vacuumize, keeps pressure inside the tank to be 0 .01-0 .02MPa and maintain 15min, take out mixture；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains sheet profile within precompressed 6 minutes in the case where pressure is 1.7-1.9Mpa, temperature is 90 DEG C
The mixture prepared in step 5 is coated in plate preform surface by base, and the temperature for controlling glue spreader is 150 DEG C, coated weight is
120-130g/m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge to obtain the final product.
Compared with prior art, the present invention have it is following the utility model has the advantages that
The present invention using fibrous raw material source it is cheap be easy to get, natural environmental-protective realizes the recycling of resource, in preparation process
Without the substances such as heavy metal and the formaldehyde, the azo that are harmful to the human body, production process is also generated without other malicious byproducts, is used
The plate inner tight of preparation method preparation of the invention, has excellent resistance to compression folding quality, plate solidification effect is good, has
Excellent flame retardant effect, while there are also preferable antimildew and antibacterial effect, plate acid and alkali-resistance, anti-current are lost, and are applied by fiber impregnation, surface
It covers, substantially increases the waterproof performance of plate, and avoid the cracking phenomena being likely to occur in dry conditions；
The plate for the preparation for being by a series of modified Enhancement Method of cooperations of this preparation method has reached hardness height, wearability
The integrative environmentally-friendly plate of good, dimensionally stable, mould proof corrosion-resistant, waterproof anticracking and excellent fireproof performance, for substituting wildwood
Wooden to make indoor furniture, decoration, wood for fittings or outdoor platform etc., security performance economic benefit greatly improves, market
It has a extensive future.
Specific embodiment
Combined with specific embodiments below, technical scheme in the embodiment of the invention is clearly and completely described, shows
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1.
A kind of preparation method of the fire protection flame retarding denseness sheet material of the present embodiment, comprising the following steps:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
5h is kept the temperature at being 50 DEG C in temperature in addition steamer, then carries out pressure cooking 1h, is then ground using defibrator, is sent into closed pressure
Force container is kept for 10 minutes under 2Mpa air pressure, is filtered mixed material after moment opening closed container, is ground mixed material
Kneadding is rubbed with the hands, and it is 35% Adlerika 10 that 4 parts of butyl titanate, 40 parts of dehydrated alcohol, mass fraction by weight are added after drying
In the dipping solution that part, 15 parts of polyvinyl alcohol proportions are formed, stirring is impregnated 20 minutes, drained and standby；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
It impregnates for 24 hours, then washes with water in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, send
Enter high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done spare；
The 17 parts of mixing of 2 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate are added 20 according to parts by weight by step 3
Part acetone soln in, reacted 80 minutes at 45 DEG C, add 7 parts of modification of chitosan magnetic agitation 5minmin at room temperature,
Mixing speed is 200 r/min, adds 5 parts of magnalium nano-layered double hydroxides after coupling agent modified, 3 part three
Poly cyanamid, 0.1 part of metal quantum point and 0.5 part of oxo double phenoxazine arsenic 10 minutes under high velocity agitation, at being 70 DEG C in temperature into
Row ultrasonic treatment 30 minutes, cooling is spare；
Step 4: by weight crushing 7 parts of energy stones for partial size is 200 mesh particles, it is added in 5 parts of acetone and is heated to 60
DEG C, add 20 parts of polyethylene glycol 1500s, 15 portions of mannitol, the shearing dispersion 10min under 2500r/min revolving speed；Then exist
8 parts of algae clay, 5 parts of expanded graphite, 1 part of active carbon are sequentially added under 100r/min revolving speed and is added in dispersion machine disperses,
10 parts of ammonium polyphosphate, 1 part of pentaerythrite, 1 part of potassium peroxydisulfate and 0.5 part of ferric sulfate are sequentially added under 100r/min revolving speed, after
Continue the shearing dispersion 15min under 3500r/min revolving speed, then is transferred in sand mill and is sanded to 1 μm of fineness <, it is spare；
Step 5: by weight by 25 parts of lauryl methacrylates, 10 parts of 13 carbon esters of methacrylic acid, 15 parts of acryloyls
Amine, 5 parts of ethyoxyl sodium alkyl sulfates and 2 parts of APES formaldehyde condensation products are stirred in advance, then pre- are stirred to described
0.3 part of ammonium sulfate of addition in solution is mixed, 3h is then reacted at 73 DEG C, it is spare；
Step 6: the mixtures that the step of mixture prepared by 80 parts of step 1 and 4 parts three prepare are added according to parts by weight high
It in fast batch mixer, is mixed 2 minutes, the mixture for adding the preparation of 40 parts of step 2 continues to stir, then will puddle end
Material is sent into vacuum roll mill, is 60 DEG C in temperature, and it is spare to obtain pretreatment material in 25% roll-in 10 minutes repeatedly for humidity；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 10min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure impregnation
In agitator tank, 0.7MPa pressure is added to stir 30 minutes；Draining valve and the complete pressure release of gas valve are successively opened, is then opened again
It opens vacuum pump to vacuumize, keeps pressure inside the tank to be 0.02MPa and maintain 10min, take out mixture；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains plate parison within precompressed 5 minutes in the case where pressure is 1.5Mpa, temperature is 85 DEG C, it will
The mixture prepared in step 5 is coated in plate preform surface, and the temperature for controlling glue spreader is 140 DEG C, coated weight 100g/
m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge to obtain the final product.
Metal quantum point in step three in the present embodiment is prepared using following methods:
It by weight disperses the titanium dioxide of 3 parts of 100nm-200nm in 40 parts of alcohol solution, the silver nitrate of 1 part of addition,
4 parts of ethylenediamines pass sequentially through in hydrothermal reaction kettle, are kept for 10 hours in 140 DEG C, are down to room temperature and filter to obtain the final product.
Multiple molding in the present embodiment in step 8 specifically:
Will treated plate parison in moulding press, be first that 150 DEG C of pressure with 10Mpa suppresses 40s in temperature, be cooled to
130 DEG C of pressure with 6Mpa suppresses 80s, then is cooled to 110 DEG C of pressure with 2Mpa and suppresses 180s.
Magnalium nano-layered double hydroxides after coupling agent modified in the present embodiment the preparation method comprises the following steps:
3:1 weighs Al (NO in molar ratio3)3·9H2O and Mg (NO3)2·6H2O is dissolved in distilled water, is stirred evenly.At 4 DEG C
Lye is quickly instilled, pH is adjusted and is reacted 30 minutes in 9.4 ranges, is dispersed filter cake in distilled water after filtering washing, 120
It is cooled to room temperature to obtain transparent whites slurry after reacting 18 h at DEG C, centrifugal drying is finely ground to 30-40 μ by the product after drying
Then m hydrolyzes the coupling agent of mass percent concentration 15% 20 minutes at room temperature, ultrasonic wave be added with stirring it is finely ground after
Product, at 80 DEG C, after filtering, wash after reaction 1h, being dry to obtain the final product.
Modification of chitosan in the present embodiment is the NH on epoxychloropropane and chitosan2It reacts, is modified with ethylenediamine again
Ethylenediamine modified crosslinking chitosan magnetic obtained and thiourea modified, glutaraldehyde cross-linking the magnetic prepared with inverse suspension crosslinking method
The mixture that property chitosan is formed according to weight ratio 3:2.
Increasing plant extracts in the present embodiment the preparation method comprises the following steps: Dalmatian chrysanthemum, Folium Forsythia, camphortree leaf, crane grass are pressed
After crushing according to weight ratio 2:3:1:1 plus water pretreatment is made using multiple counter-current extraction, shove and vacuum concentration, wherein extracting
Time be 60min, 6 times that amount of water is plant weight, degree of extracting are 40%, extraction times are 6 times, temperature concentrated in vacuo is
45±2℃。
Expanded graphite in the present embodiment the preparation method comprises the following steps:
According to mass ratio 1:1.2:0.2:1.5, by crystalline flake graphite, nitric acid, hydrogen peroxide and phosphoric acid, temperature is that 80 points are reacted at 40 DEG C again
Clock, then the sulphur-free expanded graphite that swelling volume is 312ml/g is prepared at being 900 DEG C in swelling temperature.
Embodiment 2.
A kind of preparation method of the fire protection flame retarding denseness sheet material of the present embodiment, comprising the following steps:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
7h is kept the temperature at being 70 DEG C in temperature in addition steamer, then carries out pressure cooking 2h, is then ground using defibrator, is sent into closed pressure
Force container is kept for 10 minutes under 2Mpa air pressure, is filtered mixed material after moment opening closed container, is ground mixed material
Kneadding is rubbed with the hands, and it is 35% Adlerika 15 that 6 parts of butyl titanate, 50 parts of dehydrated alcohol, mass fraction by weight are added after drying
In the dipping solution that part, 20 parts of polyvinyl alcohol proportions are formed, stirring is impregnated 30 minutes, drained and standby；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
24-48h is impregnated in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, then is washed with water,
It is sent into high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done standby
With；
The 19 parts of mixing of 2-4 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate are added according to parts by weight for step 3
It in 30 parts of acetone soln, is reacted 120 minutes at 55 DEG C, adds 9 parts of modification of chitosan magnetic agitation at room temperature
10min, mixing speed 300r/min, add 6 parts of magnalium nano-layered double hydroxides after coupling agent modified,
5 parts of melamines, 0.2 part of metal quantum point, the double phenoxazine arsenic of 1 part of oxo and 5 parts of C9 Petropols 20 minutes under high velocity agitation
Clock carries out ultrasonic treatment 50 minutes at being 80 DEG C in temperature, and cooling is spare；
Step 4: by weight crushing 9 parts of energy stones for partial size is 200 mesh particles, it is added in 7 parts of acetone and is heated to 60
DEG C, add 60 parts of polyethylene glycol 1500s, 35 portions of mannitol, the shearing dispersion 20min under 3500r/min revolving speed；Then 200
10 parts of algae clay, 9 parts of expanded graphite, 3 parts of active carbon are sequentially added under r/min revolving speed and is added in dispersion machine disperses,
14 parts of ammonium polyphosphate, 3 parts of pentaerythrites, 2 parts of potassium peroxydisulfates and 0.9 part of ferric sulfate are sequentially added under 200 r/min revolving speeds, after
Continue the shearing dispersion 30min under 4500r/min revolving speed, then is transferred in sand mill and is sanded to 1 μm of fineness <, it is spare；
Step 5: by weight by 35 parts of lauryl methacrylates, 20 parts of 13 carbon esters of methacrylic acid, 25 parts of acryloyls
Amine, 10 parts of ethyoxyl sodium alkyl sulfates and 4 parts of APES formaldehyde condensation products are stirred in advance, then pre- are stirred to described
0.5 part of ammonium sulfate of addition in solution is mixed, 6h is then reacted at 76 DEG C, it is spare；
Step 6: the mixture that is prepared the step of mixture prepared by 90 parts of step 1,15 parts three according to parts by weight, 4 parts
Borax and 1-2 parts of zinc borate are added in high speed mixer, are mixed 2-4 minutes, add 40-50 parts of step 2 preparations
Mixture continues to stir, then the material for puddling end is sent into vacuum roll mill, is 60-70 DEG C in temperature, humidity is in 25%-
35% roll-in 10-20 minutes repeatedly, it is spare to obtain pretreatment material；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 10-20min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure leaching
In stain agitator tank, 1.5MPa pressure is added to stir 50 minutes；Draining valve and the complete pressure release of gas valve are successively opened, then again
It opens vacuum pump to vacuumize, keeps pressure inside the tank to be 0 .02MPa and maintain 20min, take out mixture；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains plate parison within precompressed 7 minutes in the case where pressure is 2.0Mpa, temperature is 95 DEG C, it will
The mixture prepared in step 5 is coated in plate preform surface, and the temperature for controlling glue spreader is 160 DEG C, coated weight 150g/
m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge to obtain the final product.
Metal quantum point in step three in the present embodiment is prepared using following methods:
It by weight disperses the titanium dioxide of 5 parts of 100nm-200nm in 50 parts of alcohol solution, the silver nitrate of 2 parts of addition,
6 parts of ethylenediamines pass sequentially through in hydrothermal reaction kettle, are kept for 14 hours in 180 DEG C, are down to room temperature and filter to obtain the final product.
Multiple molding in the present embodiment in step 8 specifically:
Will treated plate parison in moulding press, be first that 160 DEG C of pressure with 12Mpa suppresses 60s in temperature, be cooled to
140 DEG C of pressure with 8Mpa suppresses 120s, then is cooled to 120 DEG C of pressure with 4Mpa and suppresses 240s.
Magnalium nano-layered double hydroxides after coupling agent modified in the present embodiment the preparation method comprises the following steps:
3:1 weighs Al (NO in molar ratio3)3·9H2O and Mg (NO3)2·6H2O is dissolved in distilled water, is stirred evenly, at 6 DEG C
Lye is quickly instilled, pH is adjusted and is reacted within the scope of 9.4-9.6 40 minutes, disperses filter cake in distilled water after filtering washing,
It is cooled to room temperature to obtain transparent whites slurry after reacting 18 h at 120 DEG C, centrifugal drying is finely ground extremely by the product after drying
30-40 μm, the coupling agent of mass percent concentration 25% is hydrolyzed 30 minutes at room temperature then, is added with stirring in ultrasonic wave
Product after finely ground, at 90 DEG C, after filtering, wash after reaction 2h, being dry to obtain the final product.
Modification of chitosan in the present embodiment is the NH on epoxychloropropane and chitosan2It reacts, is modified with ethylenediamine again
Ethylenediamine modified crosslinking chitosan magnetic obtained and thiourea modified, glutaraldehyde cross-linking the magnetic prepared with inverse suspension crosslinking method
The mixture that property chitosan is formed according to weight ratio 3:2.
Increasing plant extracts in the present embodiment the preparation method comprises the following steps: Dalmatian chrysanthemum, Folium Forsythia, camphortree leaf, crane grass are pressed
After crushing according to weight ratio 2:3:1:1 plus water pretreatment is made using multiple counter-current extraction, shove and vacuum concentration, wherein extracting
Time be 60min, 6 times that amount of water is plant weight, degree of extracting are 40%, extraction times are 6 times, temperature concentrated in vacuo is
45±2℃。
Expanded graphite in the present embodiment the preparation method comprises the following steps:
According to mass ratio 1:1.2:0.2:1.5, by crystalline flake graphite, nitric acid, hydrogen peroxide and phosphoric acid, temperature is that 80 points are reacted at 40 DEG C again
Clock, then the sulphur-free expanded graphite that swelling volume is 312ml/g is prepared at being 900 DEG C in swelling temperature.
Embodiment 3.
A kind of preparation method of the fire protection flame retarding denseness sheet material of the present embodiment, comprising the following steps:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
6h is kept the temperature at being 60 DEG C in temperature in addition steamer, then carries out pressure cooking 1.5h, is then ground using defibrator, feeding is closed
Pressure vessel is kept for 10 minutes under 2Mpa air pressure, is filtered mixed material after moment opening closed container, is carried out to mixed material
Rubbing is rolled, it is 35% Adlerika that 5 parts of butyl titanate, 45 parts of dehydrated alcohol, mass fraction by weight are added after drying
In the dipping solution of 12 parts, 18 parts of polyvinyl alcohol proportion formation, stirring is impregnated 25 minutes, drained and standby；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
36h is impregnated in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, then is washed with water, is sent
Enter high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done spare；
The 18 parts of mixing of 2-4 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate are added according to parts by weight for step 3
It in 25 parts of acetone soln, is reacted 100 minutes at 50 DEG C, adds 8 parts of modification of chitosan magnetic agitation 7min at room temperature,
Mixing speed is 250r/min, adds 5.5 parts of magnalium nano-layered double hydroxides after coupling agent modified, 4 parts
Melamine, 0.15 part of metal quantum point and 0.7 part of oxo double phenoxazine arsenic 15 minutes under high velocity agitation, in the case where temperature is 75 DEG C
Carry out ultrasonic treatment 40 minutes, cooling is spare；
Step 4: by weight crushing the energy stone that 8 parts of partial sizes are 2cm for partial size is 200 mesh particles, 6 parts of acetone is added
In be heated to 60 DEG C, add 40 parts of polyethylene glycol 1500s, 25 portions of mannitol, under 3000r/min revolving speed shear dispersion
15min；Then 9 parts of algae clay, 7 parts of expanded graphite, 2 parts of active carbon are sequentially added under 150r/min revolving speed and is added divides
Dissipate and disperse in machine, sequentially add 12 parts of ammonium polyphosphate, 2 parts of pentaerythrites under 150r/min revolving speed, 1.5 parts of potassium peroxydisulfates and
0.7 part of ferric sulfate continues the shearing dispersion 19min under 4000r/min revolving speed, then is transferred in sand mill and is sanded to 1 μm of fineness <,
It is spare；
Step 5: by weight by 30 parts of lauryl methacrylates, 15 parts of 13 carbon esters of methacrylic acid, 20 parts of acryloyls
Amine, 7 parts of ethyoxyl sodium alkyl sulfates and 3 parts of APES formaldehyde condensation products are stirred in advance, then pre- are stirred to described
0.4 part of ammonium sulfate of addition in solution is mixed, 4.5h is then reacted at 75 DEG C, it is spare；
Step 6: the mixtures that the step of mixture prepared by 85 parts of step 1 and 7 parts three prepare are added according to parts by weight high
It in fast batch mixer, is mixed 3 minutes, the mixture for adding the preparation of 45 parts of step 2 continues to stir, then will puddle end
Material is sent into vacuum roll mill, is 65 DEG C in temperature, and it is spare to obtain pretreatment material in 30% roll-in 15 minutes repeatedly for humidity；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 15min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure impregnation
In agitator tank, 1.1MPa pressure is added to stir 40 minutes；Draining valve and the complete pressure release of gas valve are successively opened, is then opened again
It opens vacuum pump to vacuumize, keeps pressure inside the tank to be 0 .01-0 .02MPa and maintain 15min, take out mixture；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains sheet profile within precompressed 6 minutes in the case where pressure is 1.7-1.9Mpa, temperature is 90 DEG C
The mixture prepared in step 5 is coated in plate preform surface by base, and the temperature for controlling glue spreader is 150 DEG C, coated weight is
120-130g/m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge to obtain the final product.
Metal quantum point in step three in the present embodiment is prepared using following methods:
It by weight disperses the titanium dioxide of 4 parts of 100nm-200nm in 45 parts of alcohol solution, 1.5 parts of nitric acid is added
Silver, 5 parts of ethylenediamines pass sequentially through in hydrothermal reaction kettle, are kept for 12 hours in 160 DEG C, are down to room temperature and filter to obtain the final product.
Multiple molding in the present embodiment in step 8 specifically:
Will treated plate parison in moulding press, be first that 155 DEG C of pressure with 11Mpa suppresses 50s in temperature, be cooled to
135 DEG C of pressure with 7Mpa suppresses 100s, then is cooled to 115 DEG C of pressure with 3Mpa and suppresses 210s.
Magnalium nano-layered double hydroxides after coupling agent modified in the present embodiment the preparation method comprises the following steps:
3:1 weighs Al (NO in molar ratio3)3·9H2O and Mg (NO3)2·6H2O is dissolved in distilled water, is stirred evenly.At 4-6 DEG C
It is lower quickly to instill lye, it adjusts pH and is reacted 35 minutes in 9.5 ranges, disperse filter cake in distilled water after filtering washing,
It is cooled to room temperature to obtain transparent whites slurry after reacting 18 h at 120 DEG C, centrifugal drying is finely ground to 30- by the product after drying
40 μm, the coupling agent of mass percent concentration 20% is hydrolyzed 25 minutes at room temperature then, is added with stirring in ultrasonic wave finely ground
Product afterwards, at 85 DEG C, after filtering, wash after reaction 1.5h, being dry to obtain the final product.
Modification of chitosan in the present embodiment is the NH on epoxychloropropane and chitosan2It reacts, is modified with ethylenediamine again
Ethylenediamine modified crosslinking chitosan magnetic obtained and thiourea modified, glutaraldehyde cross-linking the magnetic prepared with inverse suspension crosslinking method
The mixture that property chitosan is formed according to weight ratio 3:2.
Increasing plant extracts in the present embodiment the preparation method comprises the following steps: Dalmatian chrysanthemum, Folium Forsythia, camphortree leaf, crane grass are pressed
After crushing according to weight ratio 2:3:1:1 plus water pretreatment is made using multiple counter-current extraction, shove and vacuum concentration, wherein extracting
Time be 60min, 6 times that amount of water is plant weight, degree of extracting are 40%, extraction times are 6 times, temperature concentrated in vacuo is
45±2℃。
Expanded graphite in the present embodiment the preparation method comprises the following steps:
According to mass ratio 1:1.2:0.2:1.5, by crystalline flake graphite, nitric acid, hydrogen peroxide and phosphoric acid, temperature is that 80 points are reacted at 40 DEG C again
Clock, then the sulphur-free expanded graphite that swelling volume is 312ml/g is prepared at being 900 DEG C in swelling temperature.
Implementation result:
In order to verify implementation result of the invention, performance is carried out to the plate and plate in the prior art that prepare in the present embodiment
Index comparison, performance test methods use GB/T 11718-1999, GB/T1936.1-91, GB/T14019-92, referring to GB/
T18261-2000 " test method that mould inhibitor prevents and treats timber mould and Stain fungi " carries out fungicidal properties, and test concrete outcome is such as
Following table:
| Test index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Bending strength (MPa) | 41.3 | 39.4 | 42.1 | 27.8 |
| Density variation (%) | 0.34 | 0.41 | 0.24 | 1.2 |
| Thickness swelling rate (%) | 1.25 | 1.31 | 1.12 | 3.5 |
| Surface bonding strength (MPa) | 2.81 | 3.12 | 3.24 | 2.10 |
| Mould proof preventive effect (%) | 98 | 97 | 93 | 24 |
The bending strength of the plate of 1-3 of embodiment of the present invention preparation is close relative to comparative example highest promotion 51.4% as seen from the above table
Degree deviation reduces 80%, and thickness swelling rate reduces 68%, and surface bonding strength improves 54.2%, and mould proof preventive effect is promoted
More than 3 times, the contact surface of analyzing its reason present invention using base fiber and reinforcing fibre mixing cuttage, between increase fiber
Product, realizes preferable felt properties, is mixed in a certain proportion, and is conducive to the density and intensity that improve composite floor substrate, right
Base fiber carries out boiling, pressurization, rubbing, effectively increases the eduction rate of fiber, while can have by the maceration extract of proportion
Effect improves the tensile strength of of base fiber itself, its compatible degree between other substances is improved, for wood shavings, paperboard fibres
Further processing it is modified, sterilization can be effectively played and bleach and utmostly extract wherein fiber, realize the weight of resource
It is multiple to utilize；
Step 3 is the NH on epoxychloropropane and chitosan by the way that modification of chitosan is added simultaneously2Reaction is changed with ethylenediamine again
Property made from ethylenediamine modified crosslinking chitosan magnetic and with inverse suspension crosslinking method prepare it is thiourea modified, glutaraldehyde cross-linking
The mixture that chitosan magnetic is formed according to weight ratio 2:3, one side allow the binder of preparation is more uniform to be distributed
Certain filling fiber hole is played in cellulose surface, while further improving paper to prevent aqueous infiltrating agent and organic solvent
Intrusion, while there is the performance of antiacid alkali resistant, also improve the thermal stability of chitosan, additionally can be with dihydroxymethyl fourth
Acid and methyl diphenylene diisocyanate synergistic effect play good cementation to fiber；The metal quantum particularly added
Point further enhances adhesion strength because of the active group and quantum effect effect on its surface；
The present invention passes through to lauryl methacrylate, 13 carbon ester of methacrylic acid, acrylamide, ethyoxyl sodium alkyl sulfate
With the combination reaction of APES formaldehyde condensation product, it is easy to immerse and reaches deep layer effect of anti-cracking inside plate, in tide
Under the conditions of wet, protecting film can be formed on plate material surface, prevent external environment to the influence inside plate material, in dry condition
Under, can effectively prevent plate, inner material condition rapidly changes and generates cracking phenomena in dry conditions, while cooperateing with step
The double phenoxazine arsenic of the oxo added in three play the excellent effect of mildew and insect proof；
The fire retardant performance index of the plate prepared in this present embodiment and plate in the prior art is as follows:
| Test index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Mean heat capacity (J/gK) | 41.3 | 39.4 | 42.1 | 27.8 |
| Smoke release (m2) | 0.56 | 0.61 | 0.59 | 1.1 |
| Remaining carbon (%) | 54.8 | 51.2 | 59.4 | 18.6 |
| Heat liberation unit (MJ/m2) | 2.1 | 2.2 | 2.4 | 33.5 |
The fire retardant performance of 1-3 of the embodiment of the present invention is superior to the prior art as can be known from the above table, step 4 preparation of the present invention
Fire-retardant additive effectively increases the flame retardant effect of plate, in step 3 by the additional Intumescent Retardant System of common flame retardant
The magnalium nano-layered double hydroxides of addition, so that the flame-retardant smoke inhibition effect of plate is greatly improved.
The index effect of comprehensive upper table simultaneously, the indices of embodiment 1-3 are although better than comparative example, embodiment
Also difference, analysis are got off between 1-3, it is seen that the selection of the content and preparation method parameter of component also has final performance
It is most important, so the innovative content selection aspect for being also embodied in each component simultaneously of the invention, certain remaining group of the present invention
Component selections and content selection are obviously also non-obvious, and those skilled in the art combine the prior art that can think easily absolutely not
It arrives.
The present invention selects different precompressed and heat pressing process in preparation method, and cooperate corresponding temperature, pressure and
Revolving speed and etc., finally ensure that the plate of preparation has the marked improvement for preparing product compared with the existing technology and preferable city
Field competitiveness.
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.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of preparation method of fire protection flame retarding denseness sheet material, which comprises the following steps:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
5-7h is kept the temperature at being 50-70 DEG C in temperature in addition steamer, then carries out pressure cooking 1-2h, is then ground, is sent using defibrator
Enter closed pressure vessel, kept for 10 minutes under 2Mpa air pressure, mixed material is filtered after moment opening closed container, to mixture
Material carries out rolling rubbing, be added after drying butyl titanate 4-6 parts by weight, 40-50 parts of dehydrated alcohol, mass fraction be
In the dipping solution that 35% 10-15 parts of Adlerika, 15-20 parts of polyvinyl alcohol proportions are formed, stirring is impregnated 20-30 minutes, drip
It does spare；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
24-48h is impregnated in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, then is washed with water,
It is sent into high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done standby
With；
Step 3 mixes 2-4 parts of dimethylolpropionic acid and 17-19 parts of methyl diphenylene diisocyanate according to parts by weight
It is added in 20-30 parts of acetone soln, is reacted 80-120 minutes at 45-55 DEG C, add 7-9 parts of modification of chitosan room temperature
Lower magnetic agitation 5min-10min, mixing speed are 200-300r/min, add the 5-6 parts of magnaliums after coupling agent modified
Nano-layered double hydroxides, 3-5 part melamine, 0.1-0.2 parts of metal quantum points and the double phenoxazine arsenic of 0.5-1 parts of oxos
10-20 minutes under high velocity agitation, ultrasonic treatment is carried out 30-50 minutes at being 70-80 DEG C in temperature, cooling is spare；
It is described it is coupling agent modified after magnalium nano-layered double hydroxides the preparation method comprises the following steps:
3:1 weighs Al (NO in molar ratio3)3·9H2O and Mg (NO3)2·6H2O is dissolved in distilled water, is stirred evenly, at 4-6 DEG C
It is lower quickly to instill lye, it adjusts pH and is reacted within the scope of 9.4-9.6 30-40 minutes, disperse distillation for filter cake after filtering washing
In water, it is cooled to room temperature to obtain transparent whites slurry after 18 h are reacted at 120 DEG C, centrifugal drying grinds the product after drying
Carefully to 30-40 μm, then the coupling agent of mass percent concentration 15-25% is hydrolyzed 20-30 minutes at room temperature, in ultrasonic wave
It is added with stirring finely ground rear product, at 80-90 DEG C, after filtering, wash after reaction 1-2h, being dry to obtain the final product；
Step 4: by weight crushing 7-9 parts of energy stones for partial size is 200 mesh particles, it is added in 5-7 parts of acetone and is heated to
It 60 DEG C, adds 20-60 parts of polyethylene glycol 1500s, 15-35 portions of mannitol, shear dispersion under 2500-3500r/min revolving speed
10-20min；Then 8-10 parts of algae clay, 5-9 parts of expanded graphite, 1-3 are sequentially added under 100-200 r/min revolving speed
The active carbon of part, which is added in dispersion machine, to be dispersed, and 10-14 parts of ammonium polyphosphate, 1-3 parts are sequentially added under 100-200 r/min revolving speed
Pentaerythrite, 1-2 parts of potassium peroxydisulfates and 0.5-0.9 parts of ferric sulfate continue the shearing dispersion 15- under 3500-4500r/min revolving speed
30min, then be transferred in sand mill and be sanded to 1 μm of fineness <, it is spare；
Step 5: by weight by 25-35 parts of lauryl methacrylates, 10-20 parts of 13 carbon esters of methacrylic acid, 15-25
Part acrylamide, 5-10 parts of ethyoxyl sodium alkyl sulfates and 2-4 parts of APES formaldehyde condensation products are stirred in advance,
0 .3-0.5 parts of ammonium sulfate is added into the pre- agitating solution again, 3-6h is then reacted at 73-76 DEG C, it is spare；
Step 6: the mixture prepared 80-90 parts of step 1 according to parts by weight and three mixtures prepared the step of 4-10 parts
It is added in high speed mixer, is mixed 2-4 minutes, the mixture for adding the preparation of 40-50 parts of step 2 continues to stir, then will
The material for puddling end is sent into vacuum roll mill, is 60-70 DEG C in temperature, and humidity is at roll-in 10-20 points repeatedly of 25%-35%
It is spare to obtain pretreatment material for clock；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 10-20min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure leaching
In stain agitator tank, 0.7-1.5MPa pressure is added to stir 30-50 minutes；Draining valve and the complete pressure release of gas valve are successively opened,
Then it is again turned on vacuum pump to vacuumize, keeps pressure inside the tank to be 0 .01-0 .02MPa and maintain 10-20min, take out mixing
Object；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains plate within precompressed 5-7 minutes in the case where pressure is 1.5-2.0Mpa, temperature is 85-95 DEG C
Material parison, by the mixture prepared in step 5 be coated in plate preform surface, control glue spreader temperature be 140-160 DEG C,
Coated weight is 100-150g/m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge i.e.
?.
2. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the step 3
In metal quantum point be prepared using following methods:
It by weight disperses the titanium dioxide of 3-5 parts of 100nm-200nm in 40-50 parts of alcohol solution, is added 1-2 parts
Silver nitrate, 4-6 a part ethylenediamine pass sequentially through in hydrothermal reaction kettle, are kept for 10-14 hours in 140-180 DEG C, are down to room temperature mistake
It filters to obtain the final product.
3. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the step 8
In multiple molding specifically:
Will treated plate parison in moulding press, be first that the 150-160 DEG C of pressure with 10-12Mpa suppresses 40- in temperature
60s is cooled to the 130-140 DEG C of pressure with 6-8Mpa and suppresses 80-120s, then is cooled to the 110-120 DEG C of pressure with 2-4Mpa
Suppress 180-240s.
4. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the modification
Chitosan is the NH on epoxychloropropane and chitosan2It reacts, is magnetic with the modified ethylenediamine modified crosslinking obtained of ethylenediamine again
Chitosan and thiourea modified, glutaraldehyde cross-linking the chitosan magnetic prepared with inverse suspension crosslinking method are according to weight ratio 3:2 group
At mixture.
5. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the increasing
Plant extracts the preparation method comprises the following steps: by Dalmatian chrysanthemum, Folium Forsythia, camphortree leaf, crane grass according to weight ratio 2:3:1:1 crush after plus water
Pretreatment is made using multiple counter-current extraction, shove and vacuum concentration, wherein the time extracted is 60min, amount of water is plant
6 times of object weight, degree of extracting be 40%, extraction times are 6 times, temperature concentrated in vacuo is 45 ± 2 DEG C.
6. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the expansion
Graphite production processes are as follows:
According to mass ratio 1:1.2:0.2:1.5, by crystalline flake graphite, nitric acid, hydrogen peroxide and phosphoric acid, temperature is that 80 points are reacted at 40 DEG C again
Clock, then the sulphur-free expanded graphite that swelling volume is 312ml/g is prepared at being 900 DEG C in swelling temperature.
7. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the step 3
Are as follows:
20-30 is added in the 17-19 parts of mixing of 2-4 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate according to parts by weight
Part acetone soln in, reacted 80-120 minutes at 45-55 DEG C, adding 7-9 parts of modification of chitosan, magnetic force stirs at room temperature
5min-10min is mixed, mixing speed is 200-300r/min, adds the 5-6 parts of magnalium nano lamellars after coupling agent modified
The double phenoxazine arsenic of double-metal hydroxide, 3-5 part melamine, 0.1-0.2 parts of metal quantum points, 0.5-1 parts of oxos and 3-5 parts
C9 Petropols 10-20 minutes under high velocity agitation, ultrasonic treatment is carried out 30-50 minutes at being 70-80 DEG C in temperature, cooling is standby
With.
8. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that the step 6
Are as follows:
The mixture that is prepared according to parts by weight by the step of mixture prepared by 80-90 parts of step 1,7-15 parts three, 2-4 parts
Borax and 1-2 parts of zinc borate are added in high speed mixer, are mixed 2-4 minutes, add 40-50 parts of step 2 preparations
Mixture continues to stir, then the material for puddling end is sent into vacuum roll mill, is 60-70 DEG C in temperature, humidity is in 25%-
35% roll-in 10-20 minutes repeatedly, it is spare to obtain pretreatment material.
9. a kind of preparation method of fire protection flame retarding denseness sheet material according to claim 1, which is characterized in that including following step
It is rapid:
Agriculture waste stalk, the wooden factory are processed in discarded heel addition pulverizer and are crushed by step 1, mixing increasing property plant extracts
6h is kept the temperature at being 60 DEG C in temperature in addition steamer, then carries out pressure cooking 1.5h, is then ground using defibrator, feeding is closed
Pressure vessel is kept for 10 minutes under 2Mpa air pressure, is filtered mixed material after moment opening closed container, is carried out to mixed material
Rubbing is rolled, it is 35% Adlerika that 5 parts of butyl titanate, 45 parts of dehydrated alcohol, mass fraction by weight are added after drying
In the dipping solution of 12 parts, 18 parts of polyvinyl alcohol proportion formation, stirring is impregnated 25 minutes, drained and standby；
Wood shavings, paperboard fibres are crushed, 50 parts of water, 20 parts of the soda bath of mass concentration 3%, second by weight are added by step 2
36h is impregnated in the modified mixture that 5 parts of alcohol, 15 parts of hydrogen peroxide solution that mass concentration is 15% match, then is washed with water, is sent
Enter high speed dissociation device to be dissociated, the revolving speed of the high speed dissociation device is not less than 6000r/min, and dissociation end gas is done spare；
The 18 parts of mixing of 2-4 parts of dimethylolpropionic acid and methyl diphenylene diisocyanate are added according to parts by weight for step 3
It in 25 parts of acetone soln, is reacted 100 minutes at 50 DEG C, adds 8 parts of modification of chitosan magnetic agitation 7min at room temperature,
Mixing speed is 250r/min, adds 5.5 parts of magnalium nano-layered double hydroxides after coupling agent modified, 4 parts
Melamine, 0.15 part of metal quantum point and 0.7 part of oxo double phenoxazine arsenic 15 minutes under high velocity agitation, in the case where temperature is 75 DEG C
Carry out ultrasonic treatment 40 minutes, cooling is spare；
Step 4: by weight crushing the energy stone that 8 parts of partial sizes are 2cm for partial size is 200 mesh particles, 6 parts of acetone is added
In be heated to 60 DEG C, add 40 parts of polyethylene glycol 1500s, 25 portions of mannitol, under 3000r/min revolving speed shear dispersion
15min；Then 9 parts of algae clay, 7 parts of expanded graphite, 2 parts of active carbon are sequentially added under 150r/min revolving speed and is added divides
Dissipate and disperse in machine, sequentially add 12 parts of ammonium polyphosphate, 2 parts of pentaerythrites under 150r/min revolving speed, 1.5 parts of potassium peroxydisulfates and
0.7 part of ferric sulfate continues the shearing dispersion 19min under 4000r/min revolving speed, then is transferred in sand mill and is sanded to 1 μm of fineness <,
It is spare；
Step 5: by weight by 30 parts of lauryl methacrylates, 15 parts of 13 carbon esters of methacrylic acid, 20 parts of acryloyls
Amine, 7 parts of ethyoxyl sodium alkyl sulfates and 3 parts of APES formaldehyde condensation products are stirred in advance, then pre- are stirred to described
0.4 part of ammonium sulfate of addition in solution is mixed, 4.5h is then reacted at 75 DEG C, it is spare；
Step 6: the mixtures that the step of mixture prepared by 85 parts of step 1 and 7 parts three prepare are added according to parts by weight high
It in fast batch mixer, is mixed 3 minutes, the mixture for adding the preparation of 45 parts of step 2 continues to stir, then will puddle end
Material is sent into vacuum roll mill, is 65 DEG C in temperature, and it is spare to obtain pretreatment material in 30% roll-in 15 minutes repeatedly for humidity；
Step 7: pretreatment material is fitted into vacuum pressure impregnation agitator tank, opens vacuum pump and vacuumize, keep tank internal pressure
Power is 0.01MPa and maintains 15min；Liquid flowing valve is opened, the mixture of step 4 preparation is pumped into vacuum pressure impregnation
In agitator tank, 1.1MPa pressure is added to stir 40 minutes；Draining valve and the complete pressure release of gas valve are successively opened, is then opened again
It opens vacuum pump to vacuumize, keeps pressure inside the tank to be 0 .01-0 .02MPa and maintain 15min, take out mixture；
Step 8: the mixture of step 7 preparation is sent into plate spreading machine, when formation even density stabilization, thickness on mesh belt
After consistent slab, pre- press operation is carried out, obtains sheet profile within precompressed 6 minutes in the case where pressure is 1.7-1.9Mpa, temperature is 90 DEG C
The mixture prepared in step 5 is coated in plate preform surface by base, and the temperature for controlling glue spreader is 150 DEG C, coated weight is
120-130g/m2, treated plate parison is sent into moulding press after being repeatedly molded after taking out slab cutting edge to obtain the final product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112549224A (en) * | 2020-11-28 | 2021-03-26 | 浙江农林大学 | Method for manufacturing colored super-hydrophobic bamboo wood |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE50302845D1 (en) * | 2002-10-04 | 2006-05-18 | Basf Ag | METHOD FOR IMPROVING THE SURFACE HARDENESS OF A WOODEN BODY WITH AN AQUEOUS SOLUTION OF AN IMPREGNATION AGENT |
| CN102897757A (en) * | 2012-10-16 | 2013-01-30 | 清华大学 | Preparation method for single-layered graphene oxide |
| CN105566595A (en) * | 2015-12-29 | 2016-05-11 | 优美特（北京）环境材料科技股份公司 | Aqueous polyurethane emulsion used for polar surface coating, and preparation method thereof |
| CN105734042A (en) * | 2016-05-04 | 2016-07-06 | 厦门大学嘉庚学院 | Method for preparing photocatalysis type immobilized nitrogen and phosphorus removal granules |
| CN107030840A (en) * | 2017-05-27 | 2017-08-11 | 湖北中能木业有限公司 | A kind of method of utilization wood leftover material and stalk making artificial plate |
-
2018
- 2018-10-17 CN CN201811208169.0A patent/CN109278151A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE50302845D1 (en) * | 2002-10-04 | 2006-05-18 | Basf Ag | METHOD FOR IMPROVING THE SURFACE HARDENESS OF A WOODEN BODY WITH AN AQUEOUS SOLUTION OF AN IMPREGNATION AGENT |
| CN102897757A (en) * | 2012-10-16 | 2013-01-30 | 清华大学 | Preparation method for single-layered graphene oxide |
| CN105566595A (en) * | 2015-12-29 | 2016-05-11 | 优美特（北京）环境材料科技股份公司 | Aqueous polyurethane emulsion used for polar surface coating, and preparation method thereof |
| CN105734042A (en) * | 2016-05-04 | 2016-07-06 | 厦门大学嘉庚学院 | Method for preparing photocatalysis type immobilized nitrogen and phosphorus removal granules |
| CN107030840A (en) * | 2017-05-27 | 2017-08-11 | 湖北中能木业有限公司 | A kind of method of utilization wood leftover material and stalk making artificial plate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112549224A (en) * | 2020-11-28 | 2021-03-26 | 浙江农林大学 | Method for manufacturing colored super-hydrophobic bamboo wood |
| CN112549224B (en) * | 2020-11-28 | 2022-03-04 | 浙江农林大学 | Method for manufacturing colored super-hydrophobic bamboo wood |
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