CN109825101A - Polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material and preparation method thereof - Google Patents
Polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material and preparation method thereof Download PDFInfo
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- CN109825101A CN109825101A CN201910021718.1A CN201910021718A CN109825101A CN 109825101 A CN109825101 A CN 109825101A CN 201910021718 A CN201910021718 A CN 201910021718A CN 109825101 A CN109825101 A CN 109825101A
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Abstract
The present invention provides polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite materials and preparation method thereof, are related to architectural decoration material field.The preparation method of composite material in flask the following steps are included: be added palm oil polyalcohol, toluene di-isocyanate(TDI), dihydromethyl propionic acid, after being stirred to react, is cooled to room temperature to obtain base polyurethane prepolymer for use as spare；Base polyurethane prepolymer for use as and phenolic resin are added in single-necked flask, ethylenediamine is then added, is quickly stirred to react, carbon forming agent is then added, it is spare to obtain glue；Glue, corn stalk fiber and flyash are mixed, pour into mold curing molding up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.The polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material that the present invention is prepared has good mechanical property, thermal insulation property and fire protecting performance.
Description
Technical field
The present invention relates to architectural decoration material fields, prevent fires more particularly to polyurethane/phenolic aldehyde resin based high-temp-resistant compound
Material and preparation method thereof.
Background technique
Industrial production and living environment at this stage, the requirement of External Wall performance of heat protective material and technology are continuously increased,
In continuous R&D process, China's external-wall heat-insulation material and technology are rapidly developed, building exterior wall heat preserving technology in new building and
It is largely used in existing building, the research and development of external-wall heat-insulation material has become most important in China's building trade grind
Study carefully one of project.External-wall heat-insulation material is there are biggish fire safety evaluating hidden danger, and the fire incident of initiation continues to increase, with house
The requirement continuous improvement of safety, external-wall heat-insulation material and technology have become the most important thing of building trade.With environmental pollution
Continuous aggravation, external-wall heat-insulation material should meet energy-saving and emission-reduction, have safety again.Therefore, the present invention has studied poly- ammonia
Ester/phenolic resin based high-temp-resistant Flameproof composite material preparation method, the polyurethane/phenolic aldehyde resin based high-temp-resistant being prepared are anti-
Fiery composite material has good mechanical property, thermal insulation property and fire protecting performance.
Summary of the invention
Technical problems to be solved:
The purpose of the present invention is to solve the problem of mentioning in background technique and in the prior art insufficient, poly- ammonia is provided
Ester/phenolic resin based high-temp-resistant Flameproof composite material preparation method.
Technical solution:
The present invention provides the preparation methods of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material, including following step
It is rapid:
Step 1: palm oil polyalcohol is added in flask, it is warming up to 60-90 DEG C, keeps the temperature 1-3h, part toluene is then added
Diisocyanate opens agitating device and reacts 1.5-3.5h, dihydromethyl propionic acid is added, keeps the temperature 20h, be cooled to room temperature and gathered
Urethane performed polymer is spare；
Step 2: base polyurethane prepolymer for use as and phenolic resin are added in single-necked flask, ethylenediamine is then added, quickly stirs
Reaction is mixed, carbon forming agent is then added, it is spare to obtain glue；
Step 3: the glue being prepared in step 2, corn stalk fiber and flyash are mixed, in 110 DEG C of dryings
1h vacuumizes 20min at 120 DEG C, pours into mold curing molding and prevents fires composite wood up to polyurethane/phenolic aldehyde resin based high-temp-resistant
Material.
Preferably, in step 1 palm oil polyalcohol the preparation method comprises the following steps: by palm oil and formic acid, 30wt% hydrogen peroxide with
The mass ratio of the material 1:3:1.5 mixing, after 65 DEG C of hydroxylating 6h, is cooled to room temperature, and removes wherein unreacted hydrogen peroxide, formic acid
With extra moisture, it is spare to obtain palm oil polyalcohol.
Preferably, the mass ratio of base polyurethane prepolymer for use as and phenolic resin is 1:1 in step 2.
Preferably, ethylenediamine and phenolic resin mass ratio are 1:15 in step 2.
Preferably, the temperature being quickly stirred to react in step 2 is 70-90 DEG C, revolving speed 300-500r/min, and the time is
5-15min。
Preferably, carbon forming agent is mixed by melamine, ammonium polyphosphate and pentaerythrite according to mass ratio 3:18:4 in step 2
It closes.
Preferably, the partial size of corn stalk fiber is 40mm in step 3, and the partial size of flyash is 80 μm.
Preferably, in step 3 curing molding technique are as follows: in 160 DEG C of solidification 2h, then be warming up to 220 DEG C of solidification 2h, so
Solidify 1h at 260 DEG C afterwards to obtain the final product.
The utility model has the advantages that
(1) present invention prepares the performed polymer of polyurethane resin, palm using palm oil polyalcohol substitution petroleum-based polyols
Oil is renewable raw materials, meets the requirement of environmental protection, and the major components fatty acids glyceride of palm oil has hydrophobicity, uses
The polyurethane of palm oil polyols preparation has good chemical and physical properties, especially has better hydrolytic resistance and heat steady
It is qualitative.
(2) present invention is prepared by mixing into charcoal according to mass ratio 3:18:4 using melamine, ammonium polyphosphate and pentaerythrite
Agent, preferable with the compatibility of matrix, under the action of carbon forming agent, the charring rate of resin matrix is high, and the carbon-coating of formation is to undulation degree
That expects is wrapped good, and material is made to have good fire protecting performance.
Specific embodiment
The following examples can make those skilled in the art that the present invention be more fully understood, but not limit this in any way
Invention.
The preparation method of polyalcohol in embodiment 1-5 and comparative example 1:
Palm oil, formic acid and 30wt% hydrogen peroxide are mixed with the mass ratio of the material 1:3:1.5, after 65 DEG C of hydroxylating 6h,
It is cooled to room temperature, removes wherein unreacted hydrogen peroxide, formic acid and extra moisture, it is spare to obtain palm oil polyalcohol.
Embodiment 1
Step 1: 46 parts of palm oil polyalcohols are added by weight in flask, be warming up to 80 DEG C, keep the temperature 1h, then plus
Enter 52 parts of toluene di-isocyanate(TDI)s, opens agitating device and react 1.5h, 16 parts of dihydromethyl propionic acids are added, keep the temperature 20h, be cooled to
It is spare that room temperature obtains base polyurethane prepolymer for use as；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 70 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 3:18:4, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 12 parts of glues, 25 parts of 4mm corn stalk fibers and 26 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
Embodiment 2
Step 1: 38 parts of palm oil polyalcohols are added by weight in flask, be warming up to 80 DEG C, keep the temperature 1h, then plus
Enter 60 parts of toluene di-isocyanate(TDI)s, opens agitating device and react 1.5h, 12 parts of dihydromethyl propionic acids are added, keep the temperature 20h, be cooled to
It is spare that room temperature obtains base polyurethane prepolymer for use as；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 90 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 3:18:4, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 18 parts of glues, 35 parts of 4mm corn stalk fibers and 18 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
Embodiment 3
Step 1: 44 parts of palm oil polyalcohols are added by weight in flask, be warming up to 80 DEG C, keep the temperature 1h, then plus
Enter 54 parts of toluene di-isocyanate(TDI)s, opens agitating device and react 1.5h, 15 parts of dihydromethyl propionic acids are added, keep the temperature 20h, be cooled to
It is spare that room temperature obtains base polyurethane prepolymer for use as；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 75 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 3:18:4, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 14 parts of glues, 27 parts of 4mm corn stalk fibers and 24 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
Embodiment 4
Step 1: 40 parts of palm oil polyalcohols are added by weight in flask, be warming up to 80 DEG C, keep the temperature 1h, then plus
Enter 58 parts of toluene di-isocyanate(TDI)s, opens agitating device and react 1.5h, 13 parts of dihydromethyl propionic acids are added, keep the temperature 20h, be cooled to
It is spare that room temperature obtains base polyurethane prepolymer for use as；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 85 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 3:18:4, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 16 parts of glues, 33 parts of 4mm corn stalk fibers and 20 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
Embodiment 5
Step 1: 42 parts of palm oil polyalcohols are added by weight in flask, be warming up to 80 DEG C, keep the temperature 1h, then plus
Enter 56 parts of toluene di-isocyanate(TDI)s, opens agitating device and react 1.5h, 14 parts of dihydromethyl propionic acids are added, keep the temperature 20h, be cooled to
It is spare that room temperature obtains base polyurethane prepolymer for use as；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 80 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 3:18:4, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 15 parts of glues, 30 parts of 4mm corn stalk fibers and 22 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
Comparative example 1
This comparative example is the difference from embodiment 1 is that carbon forming agent is different.Specifically:
Step 1: 46 parts of palm oil polyalcohols are added by weight in flask, be warming up to 80 DEG C, keep the temperature 1h, then plus
Enter 52 parts of toluene di-isocyanate(TDI)s, opens agitating device and react 1.5h, 16 parts of dihydromethyl propionic acids are added, keep the temperature 20h, be cooled to
It is spare that room temperature obtains base polyurethane prepolymer for use as；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 70 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 4:15:3, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 12 parts of glues, 25 parts of 4mm corn stalk fibers and 26 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
Comparative example 2
This comparative example is the difference from embodiment 1 is that replace palm oil polyalcohol using polyether Glycols.Specifically:
Step 1: 46 parts of palm oil polyalcohols are added by weight in flask, 80 DEG C are warming up to, keeps the temperature 1h, 52 parts of first are then added
Phenylene diisocyanate opens agitating device and reacts 1.5h, 16 parts of dihydromethyl propionic acids are added, keeps the temperature 20h, be cooled to room temperature to obtain
Base polyurethane prepolymer for use as is spare；
Step 2: base polyurethane prepolymer for use as, phenolic resin and ethylenediamine are added to single-necked flask according to mass ratio 1:1:15
In, 70 DEG C, 300r/min stirs 10min, carbon forming agent is then added, carbon forming agent is by melamine, ammonium polyphosphate and pentaerythrite
It is mixed according to mass ratio 3:18:4, stirs 10min, obtain that glue is spare, the quality of carbon forming agent is the 0.08 of resin total amount
Times；
Step 3: by be prepared in step 2 12 parts of glues, 25 parts of 4mm corn stalk fibers and 26 parts of 80 μm of fine coal
Ash mixing, vacuumizes 20min at 110 DEG C of dry 1h, 120 DEG C, pours into mold, in 160 DEG C of solidification 2h, then be warming up to 220
DEG C solidification 2h, then solidifies 1h at 260 DEG C and is formed to obtain the final product up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
The material being prepared in embodiment 1-5 and comparative example 1-2 is tested for the property:
Product Determination of conductive coefficients is according to national standard GB/T10294-2008 " Technology of Steady State Thermal Resistance of Thermal Insulating Material and in relation to the survey of characteristic
It is fixed ", product thermal coefficient is measured using plane table thermo.It is 1000 DEG C or so that Residual carbon test, which obtains flame envelope with alcohol blast burner,
Flame calculates its Residual carbon place the material in 10min is burnt in flame with weight loss method.Tensile property test reference GB/
T1040-1992, bending property test reference GB/T9341-2000, impact property test reference GB/T1843-1996.Test knot
Fruit see the table below:
1 mechanical property test result of table
| Tensile strength/MPa | Bending strength/MPa | Impact strength/kJm-2 | |
| Embodiment 1 | 20.36 | 21.58 | 29.62 |
| Embodiment 2 | 21.59 | 22.71 | 31.24 |
| Embodiment 3 | 22.18 | 23.26 | 31.69 |
| Embodiment 4 | 24.62 | 23.84 | 32.73 |
| Embodiment 5 | 25.33 | 24.57 | 35.56 |
| Comparative example 1 | 20.44 | 20.62 | 29.87 |
| Comparative example 2 | 19.89 | 21.83 | 29.15 |
2 heat-insulating and fire-proof the performance test results of table
By test result it is found that the polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material tool that the present invention is prepared
There are good mechanical property, thermal insulation property and fire protecting performance.Compatibility between ingredient is good, and comprehensive mechanical property is preferable.?
Under the action of carbon forming agent, the charring rate of resin matrix is high, and the carbon-coating of formation has material very the wrapped good of fibrous material
Good fire protecting performance.Preparation process in embodiment 5 is the optimised process in the present invention, according to preparation process system in embodiment 5
Standby obtained thermal insulation material, tensile strength 25.33MPa, bending strength 24.57MPa, impact strength 35.56kJ
m-2, thermal coefficient 0.018Wm-1·℃-1, Residual carbon 72.72%.
Claims (8)
1. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material, which comprises the following steps:
Step 1: palm oil polyalcohol is added in flask, it is warming up to 60-90 DEG C, 1-3h is kept the temperature, toluene diisocyanate is then added
Acid esters opens agitating device and reacts 1.5-3.5h, dihydromethyl propionic acid is added, keep the temperature 20h, is cooled to room temperature to obtain polyurethane pre-
Aggressiveness is spare；
Step 2: base polyurethane prepolymer for use as and phenolic resin are added in single-necked flask, ethylenediamine is then added, quickly stirring is anti-
It answers, carbon forming agent is then added, it is spare to obtain glue；
Step 3: the glue being prepared in step 2, corn stalk fiber and flyash are mixed, in 110 DEG C of dry 1h,
20min is vacuumized at 120 DEG C, pours into mold curing molding up to polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material.
2. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, palm oil polyalcohol the preparation method comprises the following steps: by palm oil and formic acid, 30wt% hydrogen peroxide with the mass ratio of the material in step 1
1:3:1.5 mixing, after 65 DEG C of hydroxylating 6h, is cooled to room temperature, and removes wherein unreacted hydrogen peroxide, formic acid and extra water
Point, it is spare to obtain palm oil polyalcohol.
3. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, the mass ratio of base polyurethane prepolymer for use as and phenolic resin is 1:1 in step 2.
4. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, ethylenediamine and phenolic resin mass ratio are 1:15 in step 2.
5. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, the temperature being quickly stirred to react in step 2 is 70-90 DEG C, revolving speed 300-500r/min, time 5-15min.
6. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, carbon forming agent is mixed by melamine, ammonium polyphosphate and pentaerythrite according to mass ratio 3:18:4 in step 2.
7. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, the partial size of corn stalk fiber is 40mm in step 3, and the partial size of flyash is 80 μm.
8. the preparation method of polyurethane/phenolic aldehyde resin based high-temp-resistant Flameproof composite material according to claim 1, feature
It is, the technique of curing molding in step 3 are as follows: in 160 DEG C of solidification 2h, then 220 DEG C of solidification 2h are warming up to, then at 260 DEG C
Solidify 1h to obtain the final product.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763344A (en) * | 2020-07-27 | 2020-10-13 | 湖南省普力达高分子新材料股份有限公司 | Production method of flame-retardant polyurethane foam material |
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2019
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111763344A (en) * | 2020-07-27 | 2020-10-13 | 湖南省普力达高分子新材料股份有限公司 | Production method of flame-retardant polyurethane foam material |
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Application publication date: 20190531 |