CN109265979A - A kind of preparation method of the compound imitated wood material of polyurethane plant fiber - Google Patents
A kind of preparation method of the compound imitated wood material of polyurethane plant fiber Download PDFInfo
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- CN109265979A CN109265979A CN201811078432.9A CN201811078432A CN109265979A CN 109265979 A CN109265979 A CN 109265979A CN 201811078432 A CN201811078432 A CN 201811078432A CN 109265979 A CN109265979 A CN 109265979A
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- wood material
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/08—Polyurethanes from polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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- Artificial Filaments (AREA)
- Chemical And Physical Treatments For Wood And The Like (AREA)
Abstract
The present invention relates to a kind of preparation methods of compound imitated wood material of polyurethane plant fiber, belong to imitated wood material preparation technical field.The phosphate extracted in krill and silane reaction are introduced silicon-containing group into phosphate by the present invention, obtain silyl phosphate, again by silyl phosphate and steam blasting fiber-reactive, and compound imitated wood material is made with this modified fibre, the degree of cross linking of imitated wood material is also improved simultaneously, since the modified fibre surface that the present invention is added is rich in silyl phosphate, it is made after imitated wood material, it is lighted in case of fire, silyl phosphate can decompose during high-temp combustion with the polyol molecule chain of polyurethane generates metaphosphoric acid, coke layer is fire retardant simultaneously, with heat-insulated oxygen barrier effect, prevent burning, polyurethane matrix thermal conductivity is set to be deteriorated, received heat is reduced, thermal decomposition rate is slack-off, to improve the flame retardant property of compound imitated wood material, it has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of compound imitated wood material of polyurethane plant fiber, belong to imitated wood material preparation skill
Art field.
Background technique
Imitated wood material refers to a kind of have and wood materials appearance, texture or even physical mechanics intensity, machining property
Similar material, in household, the certain fields such as gardens construction, logistics can replace conventional wooden material.
Traditional imitated wood material mainly includes reinforced concrete surface imitated wood material, imitation wood tube material, Wood-plastic material etc., is showed
There is the imitated wood material preparation process of preparation all to use wood material to some extent.Armored concrete imitated wood material needs log scale more
Material makees mold to obtain surface wood grain, and high production cost, and such wood-imitated products close to woodwork, possess nothing in appearance
Machine metal material performance and non-wood moral character energy, are chiefly used in large and medium-sized pseudo-classic architecture.Traditional Wood-plastic material, which then needs to add, to be greater than
Or the wood materials equal to 50% or more, the easy moisture absorption of product, waterproof performance have much room for improvement；To realize imitative wood grain effect, generally need
It to be surface modified processing after shaping, process is relatively cumbersome.
Natural timber it is widely used, be essential using material in people's production and living.But the several years, due to
The exhaustive exploitation of the forest reserves and enough protections is lacked to the existing forest reserves, causes deterioration and the water and soil of ecological environment
Be largely lost.
In recent years, polyurethane rigid foam wood-like material has become a new neck of various countries' researcher research and development
Domain.In many traditional application fields of natural timber, part is instead of timber for polyurethane rigid foam wood-like material, such as wooden
Furniture, door and window, electric appliance casing, tub, engraving finishing device, frame etc. are widely used in a variety of applications, and such material
Can follow closely, can dig, can saw, and appearance, feel, density are similar with natural timber, there are also moisture-proof, Anti-moth-eating, it is fire-retardant, without paint etc.
The characteristics of better than timber.Polyurethane rigid foam wood-like material is the structural rigid polyurethane foam of a kind of middle-high density, it
With fine foam structure, the polyurethane rigid foam plastic for synthetic wood has fine and close tough and tensile epidermis, so that this
Kind synthetic material not only has the appearance and density range of timber.But polyurethane plant fiber common at present is compounded
Imitated wood material compound imitated wood material intensity difference obtained and is hindered since conjugation is lower between plant fiber and polyurethane matrix
It is poor to fire performance.
Therefore, a kind of intensity is high and flame retardant property the is good compound imitated wood material of polyurethane plant fiber is invented to imitated wood material
Preparation technical field has positive effect.
Summary of the invention
For the compounded imitated wood material of polyurethane plant fiber common at present, due to plant fiber and polyurethane
Conjugation is lower between body, and the defect of compound imitated wood material intensity difference obtained and poor flame retardant properties provides a kind of polyurethane
The preparation method of the compound imitated wood material of plant fiber.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) internal organ under krill carapace are taken, are fitted into tissue refiner after krill internal organ and chloroform and anhydrous methanol are mixed,
Homogenized obtains homogenate；
(2) above-mentioned homogenate is put into extracting in extractor and obtains extract, then extract is put into horizontal centrifuge, be centrifuged
Processing, isolated supernatant, stratification obtains lower layer's chloroform layer, then lower layer's chloroform layer is put into Rotary Evaporators, rotation
Krill extracting solution is obtained after steaming processing；
(3) it is fitted into reaction kettle after mixing vinyltrimethoxysilane, above-mentioned krill extracting solution and aluminum nitrate, is protected in nitrogen
It under shield, discharges after being stirred to react, obtains self-control modifier, it is spare；
(4) it weighs rice straw to be put into steam blasting tank, and is passed through into steam blasting tank and is preheated to 180~200 DEG C of water
For steam until pressure reaches 2.0~2.3MPa in tank, heat-insulation pressure keeping handles the pressure release of opening steam blasting tank after 15~20min
Valve, collection obtain gas explosion stalk fibre；
(5) it is put into reaction kettle, is stirred to react after mixing above-mentioned gas explosion stalk fibre and spare self-control modifier, reaction knot
Shu Hou, it is modified straw fiber that discharging, which collects and obtains product,；
(6) according to parts by weight, 70~80 parts of polyether polyol GR-4110,1~2 part of triethylamine, 1~1 part of glycerol are weighed, 30
~40 parts of above-mentioned modified straw fibre blends are black as white material, then with 60~70 parts of poly methylene poly phenyl poly isocyanates
White material and black material are put into reaction kettle by material, 30~40 DEG C at a temperature of be stirred to react 1~2h, obtain reaction product, will be anti-
It answers product to inject mold, is placed in cold press, demoulding is after cold pressing treatment to get the compound imitated wood material of polyurethane plant fiber.
The mass ratio of krill internal organ and chloroform and anhydrous methanol as described in step (1) is 1:2:1, the temperature of homogenized
Degree is 2~4 DEG C, and the revolving speed of homogenized is 7000~8000r/min, 30~40min of time of homogenized.
The revolving speed of centrifugal treating described in step (2) is 3000~4000r/min, time of centrifugal treating is 10~
15min, time of stratification are 10~12h, and the temperature for rotating processing is 40~50 DEG C, the time for rotating processing is 30~
40min。
The mass ratio of vinyltrimethoxysilane, krill extracting solution and aluminum nitrate described in step (3) is 10:20:
1, the temperature being stirred to react is 50~60 DEG C, and the time being stirred to react is 3~4h.
Gas explosion stalk fibre described in step (5) and the mass ratio of self-control modifier are 2:3, and the temperature being stirred to react is
120~150 DEG C, the time being stirred to react is 1~2h.
The pressure of cold pressing treatment described in step (6) is 2.0~3.0MPa, and the temperature of cold pressing treatment is 40~50 DEG C,
The time of cold pressing treatment is 1~2h.
The beneficial effects of the present invention are:
(1) for the present invention using the krill internal organ rich in glycerophosphate as raw material, extraction obtains krill phosphate, then uses ethylene again
Silyl phosphate is made in base trimethoxy silane and krill phosphate extracting solution and aluminum nitrate hybrid reaction, then uses steam blasting
Stalk fibre is made, stalk fibre is modified with silyl phosphate to obtain modified fibre, finally by modified fibre and poly- ammonia
Ester is compound to be made compound imitated wood material, and the present invention introduces the phosphate extracted in krill and silane reaction into phosphate siliceous
Group obtains silyl phosphate, then by silyl phosphate and steam blasting fiber-reactive, so that silyl phosphate and plant fiber
On hydroxyls dehydrate bonding and be fixed on fiber, obtain the modified fibre that surface has silyl phosphate, and be modified with this fine
Compound imitated wood material is made in dimension, and modified fibre surface has a large amount of active groups, can crosslink between polyurethane matrix anti-
It answers, so that fiber and the mutual conjugation of polyurethane matrix improve, while the degree of cross linking of imitated wood material is also improved, so that imitation wood
The strength of materials increases, and in addition fiber surface can form the great Si-O- of bond energy in material internal due to the introducing of silicon-containing group
Si key further increases the stability of material structure, increases its intensity；
(2) it since the modified fibre surface that the present invention is added is rich in silyl phosphate, is made after imitated wood material, in case of fire
Calamity is lighted, and silyl phosphate can decompose during high-temp combustion with the polyol molecule chain of polyurethane generates metaphosphoric acid, is being fired
Metaphosphoric acid makes polyurethane foam dehydration form one layer of close carbon-coating on surface during burning, prevents oxygen and heat to polyurethane
Content is further spread, while coke layer is fire retardant, has heat-insulated oxygen barrier effect, is prevented burning, is kept polyurethane matrix thermally conductive
Property be deteriorated, received heat is reduced, and thermal decomposition rate is slack-off, to improve the flame retardant property of compound imitated wood material, has wide answer
Use prospect.
Specific embodiment
Internal organ under krill carapace are taken, are in mass ratio after 1:2:1 is mixed by krill internal organ and chloroform and anhydrous methanol
It is fitted into tissue refiner, with revolving speed 30~40min of homogenized of 7000~8000r/min under the conditions of 2~4 DEG C, obtains
Homogenate；Homogenate is put into extractor extracting and obtains extract, then extract is put into horizontal centrifuge, with 3000~
10~15min of revolving speed centrifugal treating of 4000r/min, isolated supernatant, 10~12h of stratification obtain lower layer's chloroform
Layer, then lower layer's chloroform layer is put into Rotary Evaporators, krill extraction is obtained after 30~40min of revolving processing at 40~50 DEG C
Liquid；It is packed into and reacts after in mass ratio mixing vinyltrimethoxysilane, above-mentioned krill extracting solution and aluminum nitrate for 10:20:1
In kettle, it is heated to 50~60 DEG C under nitrogen protection, discharges after being stirred to react 3~4h, obtains self-control modifier, it is spare；
Rice straw is weighed to be put into steam blasting tank, and be passed through into steam blasting tank be preheated to 180~200 DEG C vapor until
Pressure reaches 2.0~2.3MPa in tank, and heat-insulation pressure keeping handles the relief valve of opening steam blasting tank after 15~20min, collects
To gas explosion stalk fibre；It is in mass ratio to be put into reaction kettle after 2:3 is mixed by gas explosion stalk fibre and spare self-control modifier
In, 120~150 DEG C are heated to, 1~2h is stirred to react, after reaction, it is modified straw that discharging, which collects and obtains product,
Fiber；According to parts by weight, 70~80 parts of polyether polyol GR-4110,1~2 part of triethylamine, 1~2 part of glycerol are weighed, 30~
40 parts of above-mentioned modified straw fibre blends are black as white material, then with 60~70 parts of poly methylene poly phenyl poly isocyanates
White material and black material are put into reaction kettle by material, 30~40 DEG C at a temperature of be stirred to react 1~2h, obtain reaction product, will be anti-
It answers product to inject mold, is placed in cold press, be 2.0~3.0MPa in pressure, under conditions of temperature is 40~50 DEG C, at cold pressing
Demoulding is after managing 1~2h to get the compound imitated wood material of polyurethane plant fiber.
Internal organ under krill carapace are taken, are in mass ratio after 1:2:1 is mixed by krill internal organ and chloroform and anhydrous methanol
It is fitted into tissue refiner, with the revolving speed homogenized 30min of 7000r/min under the conditions of 2 DEG C, obtains homogenate；It will homogenate
Liquid is put into extracting in extractor and obtains extract, then extract is put into horizontal centrifuge, is centrifuged with the revolving speed of 3000r/min
10min is handled, isolated supernatant, stratification 10h obtains lower layer's chloroform layer, then lower layer's chloroform layer is put into rotary evaporation
In instrument, krill extracting solution is obtained after revolving processing 30min at 40 DEG C；It is in mass ratio 10:20:1 by vinyl trimethoxy
It is fitted into reaction kettle after silane, above-mentioned krill extracting solution and aluminum nitrate mixing, is heated to 50 DEG C under nitrogen protection, stirring
It discharges after reaction 3h, obtains self-control modifier, it is spare；It weighs rice straw to be put into steam blasting tank, and to steam blasting tank
In be passed through and be preheated to 180 DEG C of vapor until pressure reaches 2.0MPa in tank, heat-insulation pressure keeping handles that open steam after 15min quick-fried
The relief valve of broken tank, collection obtain gas explosion stalk fibre；It is in mass ratio by gas explosion stalk fibre and spare self-control modifier
It is put into reaction kettle after 2:3 mixing, is heated to 120 DEG C, is stirred to react 1h, after reaction, discharging collects and obtains product
As modified straw fiber；According to parts by weight, 70 parts of polyether polyol GR-4110,1 part of triethylamine, 1 part of glycerol are weighed, 30
Part above-mentioned modified straw fibre blend is as white material, will be white then with 60 parts of poly methylene poly phenyl poly isocyanates for black material
Material is put into reaction kettle with black material, 30 DEG C at a temperature of be stirred to react 1h, obtain reaction product, reaction product injected into mould
Tool, is placed in cold press, is 2.0MPa in pressure, under conditions of temperature is 40 DEG C, demoulding is after cold pressing treatment 1h to get polyurethane
The compound imitated wood material of plant fiber.
Internal organ under krill carapace are taken, are in mass ratio after 1:2:1 is mixed by krill internal organ and chloroform and anhydrous methanol
It is fitted into tissue refiner, with the revolving speed homogenized 35min of 7500r/min under the conditions of 3 DEG C, obtains homogenate；It will homogenate
Liquid is put into extracting in extractor and obtains extract, then extract is put into horizontal centrifuge, is centrifuged with the revolving speed of 3500r/min
12min is handled, isolated supernatant, stratification 11h obtains lower layer's chloroform layer, then lower layer's chloroform layer is put into rotary evaporation
In instrument, krill extracting solution is obtained after revolving processing 35min at 45 DEG C；It is in mass ratio 10:20:1 by vinyl trimethoxy
It is fitted into reaction kettle after silane, above-mentioned krill extracting solution and aluminum nitrate mixing, is heated to 55 DEG C under nitrogen protection, stirring
It discharges after reaction 3.5h, obtains self-control modifier, it is spare；It weighs rice straw to be put into steam blasting tank, and to steam blasting
It is passed through in tank and is preheated to 190 DEG C of vapor until pressure reaches 2.2MPa in tank, heat-insulation pressure keeping opens steam after handling 17min
The relief valve of cavity charge containers, collection obtain gas explosion stalk fibre；In mass ratio by gas explosion stalk fibre and spare self-control modifier
To be put into reaction kettle after 2:3 mixing, 135 DEG C are heated to, 1.5h is stirred to react, after reaction, discharging is collected and obtained
Product is modified straw fiber；According to parts by weight, weigh 75 parts of polyether polyol GR-4110,1 part of triethylamine, 1 part it is sweet
Oil, 35 parts of above-mentioned modified straw fibre blends are black as white material, then with 65 parts of poly methylene poly phenyl poly isocyanates
White material and black material are put into reaction kettle by material, 35 DEG C at a temperature of be stirred to react 1.5h, obtain reaction product, reaction produced
Object injects mold, is placed in cold press, is that 2.5MPa is demoulded after cold pressing treatment 1.5h under conditions of temperature is 45 DEG C in pressure,
Up to the compound imitated wood material of polyurethane plant fiber.
Internal organ under krill carapace are taken, are in mass ratio after 1:2:1 is mixed by krill internal organ and chloroform and anhydrous methanol
It is fitted into tissue refiner, with the revolving speed homogenized 40min of 8000r/min under the conditions of 4 DEG C, obtains homogenate；It will homogenate
Liquid is put into extracting in extractor and obtains extract, then extract is put into horizontal centrifuge, is centrifuged with the revolving speed of 4000r/min
15min is handled, isolated supernatant, stratification 12h obtains lower layer's chloroform layer, then lower layer's chloroform layer is put into rotary evaporation
In instrument, krill extracting solution is obtained after revolving processing 40min at 50 DEG C；It is in mass ratio 10:20:1 by vinyl trimethoxy
It is fitted into reaction kettle after silane, above-mentioned krill extracting solution and aluminum nitrate mixing, is heated to 60 DEG C under nitrogen protection, stirring
It discharges after reaction 4h, obtains self-control modifier, it is spare；It weighs rice straw to be put into steam blasting tank, and to steam blasting tank
In be passed through and be preheated to 200 DEG C of vapor until pressure reaches 2.3MPa in tank, heat-insulation pressure keeping handles that open steam after 20min quick-fried
The relief valve of broken tank, collection obtain gas explosion stalk fibre；It is in mass ratio by gas explosion stalk fibre and spare self-control modifier
It is put into reaction kettle after 2:3 mixing, is heated to 150 DEG C, is stirred to react 2h, after reaction, discharging collects and obtains product
As modified straw fiber；According to parts by weight, 80 parts of polyether polyol GR-4110,2 parts of triethylamines, 2 parts of glycerol are weighed, 40
Part above-mentioned modified straw fibre blend is as white material, will be white then with 70 parts of poly methylene poly phenyl poly isocyanates for black material
Material is put into reaction kettle with black material, 40 DEG C at a temperature of be stirred to react 2h, obtain reaction product, reaction product injected into mould
Tool, is placed in cold press, is 3.0MPa in pressure, under conditions of temperature is 50 DEG C, demoulding is after cold pressing treatment 2h to get polyurethane
The compound imitated wood material of plant fiber.
The compound imitated wood material of polyurethane plant fiber that comparative example is produced with Shenzhen company is as a comparison case to the present invention
The compound imitated wood material progressive of polyurethane plant fiber in the compound imitated wood material of polyurethane plant fiber obtained and comparative example
It can detect, testing result is as shown in table 1:
Test method:
Compressive strength, impact strength and bending strength test using " test methods of evaluating the properties of wood-based panels and surface decorated wood-based panels " into
Row detection.
Flame lateral spread length test is detected by the standard of GB20284-2006.
Oxygen index (OI) test is detected using oxygen index (OI) tester.
By flame retardant rating by HB, the standard that V-2, V-1 are incremented by step by step to V-0 is detected for flame retardant rating test.
1 imitated wood material performance measurement of table
High, the impact strength according to the compound imitated wood material compressive strength of above-mentioned detection data polyurethane plant fiber of the invention
Height, bending strength is high, and mechanical property is good, good flame resistance, and flame retardant rating is high, has broad application prospects.
Claims (6)
1. a kind of preparation method of the compound imitated wood material of polyurethane plant fiber, it is characterised in that specific preparation step are as follows:
(1) internal organ under krill carapace are taken, are fitted into tissue refiner after krill internal organ and chloroform and anhydrous methanol are mixed,
Homogenized obtains homogenate；
(2) above-mentioned homogenate is put into extracting in extractor and obtains extract, then extract is put into horizontal centrifuge, be centrifuged
Processing, isolated supernatant, stratification obtains lower layer's chloroform layer, then lower layer's chloroform layer is put into Rotary Evaporators, rotation
Krill extracting solution is obtained after steaming processing；
(3) it is fitted into reaction kettle after mixing vinyltrimethoxysilane, above-mentioned krill extracting solution and aluminum nitrate, is protected in nitrogen
It under shield, discharges after being stirred to react, obtains self-control modifier, it is spare；
(4) it weighs rice straw to be put into steam blasting tank, and is passed through into steam blasting tank and is preheated to 180~200 DEG C of water
For steam until pressure reaches 2.0~2.3MPa in tank, heat-insulation pressure keeping handles the pressure release of opening steam blasting tank after 15~20min
Valve, collection obtain gas explosion stalk fibre；
(5) it is put into reaction kettle, is stirred to react after mixing above-mentioned gas explosion stalk fibre and spare self-control modifier, reaction knot
Shu Hou, it is modified straw fiber that discharging, which collects and obtains product,；
(6) according to parts by weight, 70~80 parts of polyether polyol GR-4110,1~2 part of triethylamine, 1~1 part of glycerol are weighed, 30
~40 parts of above-mentioned modified straw fibre blends are black as white material, then with 60~70 parts of poly methylene poly phenyl poly isocyanates
White material and black material are put into reaction kettle by material, 30~40 DEG C at a temperature of be stirred to react 1~2h, obtain reaction product, will be anti-
It answers product to inject mold, is placed in cold press, demoulding is after cold pressing treatment to get the compound imitated wood material of polyurethane plant fiber.
2. a kind of preparation method of compound imitated wood material of polyurethane plant fiber according to claim 1, it is characterised in that:
The mass ratio of krill internal organ and chloroform and anhydrous methanol as described in step (1) is 1:2:1, and the temperature of homogenized is 2~4
DEG C, the revolving speed of homogenized is 7000~8000r/min, 30~40min of time of homogenized.
3. a kind of preparation method of compound imitated wood material of polyurethane plant fiber according to claim 1, it is characterised in that:
The revolving speed of centrifugal treating described in step (2) is 3000~4000r/min, and the time of centrifugal treating is 10~15min, is stood
The time of layering is 10~12h, and the temperature for rotating processing is 40~50 DEG C, and the time for rotating processing is 30~40min.
4. a kind of preparation method of compound imitated wood material of polyurethane plant fiber according to claim 1, it is characterised in that:
The mass ratio of vinyltrimethoxysilane, krill extracting solution and aluminum nitrate described in step (3) is 10:20:1, and stirring is anti-
The temperature answered is 50~60 DEG C, and the time being stirred to react is 3~4h.
5. a kind of preparation method of compound imitated wood material of polyurethane plant fiber according to claim 1, it is characterised in that:
Gas explosion stalk fibre described in step (5) and the mass ratio of self-control modifier are 2:3, and the temperature being stirred to react is 120~150
DEG C, the time being stirred to react is 1~2h.
6. a kind of preparation method of compound imitated wood material of polyurethane plant fiber according to claim 1, it is characterised in that:
The pressure of cold pressing treatment described in step (6) is 2.0~3.0MPa, and the temperature of cold pressing treatment is 40~50 DEG C, cold pressing treatment
Time be 1~2h.
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Application publication date: 20190125 |