CN107141443A - A kind of flame retarding polyether composition and its preparation method and application - Google Patents
A kind of flame retarding polyether composition and its preparation method and application Download PDFInfo
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- CN107141443A CN107141443A CN201710258909.0A CN201710258909A CN107141443A CN 107141443 A CN107141443 A CN 107141443A CN 201710258909 A CN201710258909 A CN 201710258909A CN 107141443 A CN107141443 A CN 107141443A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4804—Two or more polyethers of different physical or chemical nature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/50—Polyethers having heteroatoms other than oxygen
- C08G18/5075—Polyethers having heteroatoms other than oxygen having phosphorus
- C08G18/509—Polyethers having heteroatoms other than oxygen having phosphorus having nitrogen in addition to phosphorus
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/335—Polymers modified by chemical after-treatment with organic compounds containing phosphorus
- C08G65/3353—Polymers modified by chemical after-treatment with organic compounds containing phosphorus containing oxygen in addition to phosphorus
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L71/00—Compositions of polyethers obtained by reactions forming an ether link in the main chain; Compositions of derivatives of such polymers
- C08L71/02—Polyalkylene oxides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of flame retarding polyether composition, including following component in parts by weight：First 70 90 parts of PPG；Second 10 30 parts of PPG；130 150 parts of methyl diphenylene diisocyanate；10 15 parts of silicate powder；23 parts of stabilizer；First 25 parts of catalyst；0.3 6 parts of water.The flame retarding polyether composition good flame retardation effect, without addition fire retardant, storage-stable more than 6 months of product；And fray-out of flame is fast, smoke amount is small；Halogen element, good environmental protection are free of be formulated simultaneously in.Present invention also offers a kind of preparation method of flame retarding polyether composition, step is few, and flow is simple, safe operation.The present invention provides a kind of fire proofing and preparation method thereof, good flame retardation effect again, and material, which lights its rear surface, can quickly form phosphorous charing protective layer, prevent material to burn away, with the characteristics of fray-out of flame is fast, smoke amount is small；Preparation process is simple and efficient.
Description
Technical field
The present invention relates to fire proofing technical field, more particularly to a kind of flame retarding polyether composition and preparation method thereof and should
With.
Background technology
PPG (abbreviation polyethers) is by initiator (compound containing active hydrogen group) and oxirane (EO), ring
Ethylene Oxide (PO), epoxy butane (BO) etc. are made through sudden reaction in the presence of a catalyst.It is logical that PPG is usually used in manufacture
With polyurethane foam plastics, adhesive and elastomer etc., special PPG also serves as defoamer, surfactant etc..
At present, during using polyether polyols alcohol production polyurethane foam plastics, fire retardant, example be generally needed to be added
Such as TCPP, DMMP, but the product obtained haves the shortcomings that inflammable, flame retardant effect is poor；Meanwhile, flame hardly possible is extinguished, black smoke
Larger, the Storage period of preparing raw material is also shorter, typically only short 1-3 days.Once have been reported that using nitrogenous PPG, can
The problem of Storage period is short is solved, still, the problem of flame hardly possible is extinguished, black smoke is larger is still present.
The content of the invention
In order to overcome the deficiencies in the prior art, first purpose of the invention is to provide a kind of flame retarding polyether composition,
Its good flame retardation effect, without addition fire retardant, storage-stable more than 6 months of product；And fray-out of flame is fast, smoke amount is small；
Halogen element, good environmental protection are free of be formulated simultaneously in.
Second object of the present invention is to provide a kind of preparation method of flame retarding polyether composition, and step is few, flow letter
Single, processing safety is high.
Third object of the present invention is to provide a kind of fire proofing, good flame retardation effect, its surface energy after material is lighted
It is enough quickly to form phosphorous charing protective layer, prevent material to burn away, with the characteristics of fray-out of flame is fast, smoke amount is small.
Fourth object of the present invention is to provide a kind of preparation method of fire proofing, simple and efficient to handle.
First purpose of the present invention is realized using following technical scheme：
A kind of flame retarding polyether composition, including following component in parts by weight：
It is preferred that, first PPG is prepared from accordance with the following steps：
1) first by melamine polyols and dimethylamine according to mol ratio 10：10- is stirred under 1 mixing, normal temperature condition
50min, obtains the first mixture；
2) phosphate and the second catalyst are added into first mixture, stirs, is then increased to temperature
80-120 DEG C, reacted, the reaction time is 1.5-2.5h；The mass ratio of first mixture and the phosphate is 70:
30；Second catalyst is monoethanolamine manganate, and its consumption is the 1% of the phosphate quality；
3) temperature of question response system drops to less than 50 DEG C, is vacuumized under conditions of the MPa of (- 0.02)-(- 0.1), then
90-130 DEG C is warming up to, continues to vacuumize, residual monomer is removed, obtains first PPG.
It is preferred that, the mol ratio of the residual monomer of removing and first PPG is 1.8:100；Pressed when vacuumizing
Power is -0.1MPa, and the time vacuumized is 2-3h.
It is preferred that, second PPG is prepared from accordance with the following steps：
1) first by isocyanuric acid polyalcohol and dimethylamine according to mol ratio 11.6：10- is stirred under 1 mixing, normal temperature condition
50min, obtains the second mixture；
2) phosphate and the 3rd catalyst are added into second mixture, stirs, is then increased to temperature
80-120 DEG C, reacted, the reaction time is 1.5-2.5h；The mass ratio of second mixture and the phosphate is 70:
30；3rd catalyst is monoethanolamine manganate, and its consumption is the 1% of the phosphate quality；
3) question response system temperature drops to less than 50 DEG C, vacuumizes, then rises under conditions of the MPa of (- 0.02)-(- 0.1)
Temperature continues to vacuumize to 90-130 DEG C, removes residual monomer, obtains second PPG.
It is preferred that, in step 3) in, the mol ratio 2.69 of the residual monomer of removing and second PPG:100；
Pressure is -0.1MPa when vacuumizing, and the time vacuumized is 2-3h.
It is preferred that, the viscosity of first PPG is 250-350, and hydroxyl value is 100-200；Second polyethers is more
The viscosity of first alcohol is 9800-10200, and hydroxyl value is 100-200；Average grain diameter≤2 μm of the silicate powder；The stabilizer is
Surfactant containing element silicon, for example, can select the silicone oil surface for the model 84805,8545 for originating from Degussa companies
Activating agent；First catalyst is composite catalyst, and the composite catalyst is N, N', N "-three (dimethylamino-propyl)-six
Hydrogenate any combination of triazine, (dimethylamino methyl) phenol of 2,4,6- tri- and pentamethyl-diethylenetriamine.
It is preferred that, including following component in parts by weight：
Second object of the present invention is realized using following technical scheme：
A kind of preparation method of flame retarding polyether composition, is prepared from according to following steps：The polyethers of formula ratio first is more
First alcohol is added in band high speed disperser reactor, and 10-20min is stirred with 60-80r/min speed；Then formula is sequentially added
Stabilizer, water and the first catalyst of amount, are followed by stirring for 15-25min；The second PPG of formula ratio is subsequently added, after
After continuous stirring 12-18min, the silicate powder of formula ratio is added, 70-80 DEG C is warming up to, is stirred with 600-1000r/min speed
25-35min, is produced.
Third object of the present invention is realized using following technical scheme：
A kind of fire proofing, is prepared from by the flame retarding polyether composition, and isocyanates；The flame retarding polyether group
The weight ratio of compound and the isocyanates is 1：(1.3-1.5).
Fourth object of the present invention is realized using following technical scheme：
A kind of preparation method of fire proofing, is prepared from according to following steps：The flame retarding polyether composition and institute
Isocyanates mixing is stated, after stirring, in injection mould, compression molding.
In actual mechanical process, mould used can be rubber mold, can be mold base with true stone, after shaping i.e.
Obtain immitation stone plate, it is adaptable to external wall or inner wall decoration, product can also paint coloring as needed.
Compared with prior art, the beneficial effects of the present invention are：
(1) the first PPG and the second polyethers in flame retarding polyether composition provided by the present invention, preparing raw material
Polyalcohol has accessed nitrogen phosphorus (P/N) element on strand, and the two PPGs coordinate by foaming agent of water, amine is urged
Agent, foam stabilizing stabilizer, nanometer scale silicate micro mist, have synthesized the polyether composition that fire resistance reaches B2 grades.Also, formula
Fire retardant need not be added, flame retardant effect is good, storage-stable 6 months of product；Contain substantial amounts of nitrogen, phosphorus in raw material strand
Element, material lights its rear surface and quickly forms phosphorous charing protective layer, prevents foam to burn away, with fray-out of flame
It hurry up, the characteristics of smoke amount is small.Meanwhile, halogen element, good environmental protection are free of in formula.
(2) preparation method of flame retarding polyether composition provided by the present invention, step is few, and flow is simple, processing safety
It is high.
(3) fire proofing provided by the present invention, with good heat preservation and insulation and fire resistance, thermal conductivity factor is less than
24mW/m.K, oxygen index (OI) are more than 26, and fire-retardant detection has the characteristics of fray-out of flame is fast, smoke amount is small, and flame retardant rating reaches GB/
B2 grades of T8624 standards.Compared with tradition addition flame retardant combination polyethers formula, storage stability, the anti-flammability of the fire proofing
Can be more excellent with heat-insulation and heat-preservation.
(4) preparation method of fire proofing provided by the present invention, simple and efficient to handle.
Embodiment
Below, with reference to embodiment, the present invention is described further：
Embodiment 1
A kind of flame retarding polyether composition, including following component in parts by weight：First PPG (viscosity 300,
Hydroxyl value 150) 90 parts, 10 parts of the second PPG (viscosity 10000, hydroxyl value 150), stabilizer (the silicone oil surface of model 84805
Activating agent) 3 parts；Composite catalyst (N, N', N "-three (dimethylamino-propyl)-hexahydrotriazine, (the dimethylamino first of 2,4,6- tri-
Base) phenol) 5 parts；1 part of water；15 parts of silicic acid powder；130 parts of methyl diphenylene diisocyanate.
The flame retarding polyether composition is prepared from according to following steps：The PPG of formula ratio first is added band at a high speed
In disperser reactor, 20min is stirred with 60-80r/min speed；Then stabilizer, the water and of formula ratio are sequentially added
One catalyst, is followed by stirring for 20min；The second PPG of formula ratio is subsequently added, continues to stir after 15min, addition is matched somebody with somebody
The silicate powder of side's amount, is warming up to 70-80 DEG C, stirs 30min with 600-1000r/min speed, produces.
Wherein, the first PPG is prepared from according to following steps：
1) melamine polyols 840g (mean molecule quantity is 500) and dimethylamine 18.8g (two is added in four-hole boiling flask
Methylamine is 40% aqueous solution), thermometer and agitator are connected, 20min is continuously stirred at normal temperatures.
2) and then phosphate 360g, monoethanolamine mangaic acid salt catalyst 3.6g are added, under stirring, is warming up to 80-100
DEG C, react 2h.
3) reaction system is cooled to after 50 DEG C, it is that -0.1MPa, temperature are 100 DEG C -130 DEG C to connect condenser in pressure
Under the conditions of vacuumize 2h, remove residual monomer, you can melamine polyols phosphate ester product.Wherein, the remnants of removing are single
The mol ratio 1.8 of body and melamine polyols phosphate:100.
Second PPG is prepared from according to following steps：
1) isocyanuric acid polyalcohol 840g (mean molecule quantity is 600) and dimethylamine (dimethylamine are added in four-hole boiling flask
For 40% aqueous solution) 13.6g, thermometer and agitator are connected, 20min is continuously stirred at normal temperatures.
2) and then phosphate 360g, monoethanolamine mangaic acid salt catalyst 3.6g are added, under stirring, is warming up to 80-100
DEG C, react 2h.
3) reaction system is cooled to after 50 DEG C, it is that -0.1MPa, temperature are 100 DEG C -130 DEG C to connect condenser in pressure
Under the conditions of vacuumize 2h, remove residual monomer, you can isocyanuric acid polyolphosphateester product.Wherein, the remnants of removing are single
The mol ratio 1.8 of body and isocyanuric acid polyolphosphateester:100.
The formula system of embodiment 1 is adapted to the higher immitation stone plate of high pressure foaming machine production density.In this system, add simultaneously
First PPG and the second PPG, play synergy between the two, the first PPG be reduced black smoke,
Regulation system viscosity is acted on；Second PPG, which has, preferably to be obstructed flame, shortens burning time, reduce black smoke, improve pressure
Contracting intensity is acted on.Also, the silicate micro mist in system can reduce the generation of black smoke, shorten burning time；And diphenylmethyl
Alkane diisocyanate then plays crosslinking, solidification well.
Embodiment 2
A kind of flame retarding polyether composition, including following component in parts by weight：First PPG (viscosity 300,
Hydroxyl value 150) 60 parts, 30 parts of the second PPG (viscosity 10000, hydroxyl value 150), stabilizer (the silicone oil table of model 8545
Face activating agent) 2.5 parts；3.5 parts of composite catalyst (2,4,6- tri- (dimethylamino methyl) phenol, pentamethyl-diethylenetriamine)；
5 parts of water；10 parts of silicate powder；130 parts of methyl diphenylene diisocyanate.
The flame retarding polyether composition is prepared from according to following steps：The PPG of formula ratio first is added band at a high speed
In disperser reactor, 15min is stirred with 60-80r/min speed；Then stabilizer, the water and of formula ratio are sequentially added
One catalyst, is followed by stirring for 25min；The second PPG of formula ratio is subsequently added, continues to stir after 12min, addition is matched somebody with somebody
The silicate powder of side's amount, is warming up to 70-80 DEG C, stirs 25min with 600-1000r/min speed, produces.
Wherein, the first PPG is prepared from according to following steps：
1) melamine polyols 840g (mean molecule quantity is 800) and dimethylamine (dimethylamine are added in four-hole boiling flask
For 40% aqueous solution) 18.8g, thermometer and agitator are connected, 50min is continuously stirred at normal temperatures.
2) and then phosphate 320g, monoethanolamine mangaic acid salt catalyst 5g are added, under stirring, is warming up to 100-120
DEG C, react 2.5h.
3) reaction system is cooled to after 50 DEG C, it is that -0.1MPa, temperature are 110 DEG C -130 DEG C to connect condenser in pressure
Under the conditions of vacuumize 3h, remove residual monomer, you can melamine polyols phosphate ester product.Wherein, the remnants of removing are single
The mol ratio 2.1 of body and melamine polyols phosphate:100.
Second PPG is prepared from according to following steps：
1) isocyanuric acid polyalcohol 840g (mean molecule quantity is 1300) and dimethylamine (dimethylamine are added in four-hole boiling flask
For 40% aqueous solution) 13.6g, thermometer and agitator are connected, 50min is continuously stirred at normal temperatures.
2) and then phosphate 320g, monoethanolamine mangaic acid salt catalyst 5g are added, under stirring, is warming up to 100-120
DEG C, react 2.5h.
3) reaction system is cooled to after 50 DEG C, it is that -0.1MPa, temperature are 110 DEG C -130 DEG C to connect condenser in pressure
Under the conditions of vacuumize 3h, remove residual monomer, you can isocyanuric acid polyolphosphateester product.Wherein, the remnants of removing are single
The mol ratio 2.1 of body and isocyanuric acid polyolphosphateester:100.
The formula system of embodiment 2 is adapted to the relatively low imitative stone sheet material of low-pressure blowing machine production density.
Embodiment 3
The difference of embodiment 3 and embodiment 1 is that the first PPG is prepared from according to following steps：
1) melamine polyols 840g (mean molecule quantity is 600) and dimethylamine (dimethylamine are added in four-hole boiling flask
For 40% aqueous solution) 18.8g, thermometer and agitator are connected, 25min is continuously stirred at normal temperatures.
2) and then phosphate 400g, monoethanolamine mangaic acid salt catalyst 4g are added, under stirring, is warming up to 90-110
DEG C, react 2.5h.
3) reaction system is cooled to after 50 DEG C, it is that -0.05MPa, temperature are 100 DEG C -120 DEG C to connect condenser in pressure
Under the conditions of vacuumize 2.5h, remove residual monomer, you can melamine polyols phosphate ester product.Wherein, the remnants of removing
The mol ratio 1.9 of monomer and melamine polyols phosphate:100.
Embodiment 4
The difference of embodiment 4 and embodiment 1 is that the second PPG is prepared from according to following steps：
1) isocyanuric acid polyalcohol 840g (mean molecule quantity is 1000) and dimethylamine (dimethylamine are added in four-hole boiling flask
For 40% aqueous solution) 13.6g, thermometer and agitator are connected, 25min is continuously stirred at normal temperatures.
2) and then phosphate 400g, monoethanolamine mangaic acid salt catalyst 4g are added, under stirring, is warming up to 90-110
DEG C, react 2.5h.
3) reaction system is cooled to after 50 DEG C, it is that -0.05MPa, temperature are 100 DEG C -120 DEG C to connect condenser in pressure
Under the conditions of vacuumize 2.5h, remove residual monomer, you can isocyanuric acid polyolphosphateester product.Wherein, the remnants of removing
The mol ratio 1.9 of monomer and isocyanuric acid polyolphosphateester:100.
Embodiment 5
The difference of embodiment 5 and embodiment 1 is：The formula of flame retarding polyether composition is different, including according to weight
The following component of part meter：First 75 parts of PPG, the second 25 parts of PPG, 2.5 parts of stabilizer；Composite catalyst
4 parts of (N, N', N "-three (dimethylamino-propyl)-hexahydrotriazine, 2,4,6- tri- (dimethylamino methyl) phenol)；4 parts of water；Silicon
Sour 12 parts of powder；138 parts of methyl diphenylene diisocyanate.
Flame retardant effect is evaluated and tested
Using traditional test methods, to unitary system：First PPG, the second PPG, and complex
System：The flame retardant effect of embodiment 1-5 flame retarding polyether composition is tested, and test result is as described below：
First PPG：Foamy body is high, and burning fuming amount is minimum, the foam being made using the first PPG
More than compressive strength 180kPa；Viscosity is smaller (300mPa.s), available for adjustment system viscosity；The first polyether polyols are used alone
Stop working after 15~20s of foam combustion that alcohol is made, smoke amount is more with respect to the second PPG.
Second PPG：Carburization zone quickly is formed with shortening burning time, meeting when fire burns, effectively isolation fire
Flame, the characteristics of smoke amount is few；The foam being made using the second PPG, its combustion process is formed on surface carbonize quickly
Layer, can completely cut off flame and deeply burn, reduce black smoke, compressive strength >=200kPa；But the second PPG system is used alone
Standby foam, viscosity is larger (＞ 1000mPa.s), generally to coordinate the first PPG to use, and 8~12s of burning is used alone
After stop working.
Embodiment 1-5 flame retarding polyether composition：Compound, the body using the first PPG and the second PPG
It is to stop working after 400~700mPa.s of viscosity, compressive strength >=200kPa, 6~10s of burning time.In this compound system, first gathers
Ethoxylated polyhydric alcohol and the second PPG are mutually cooperateed with, compared with unitary system, and flame retardant effect is more preferable, with appropriate viscosity and combustion
Advantage of the burning time compared with compressive strength short, that smoke amount is few, higher etc..
It will be apparent to those skilled in the art that technical scheme that can be as described above and design, make other various
It is corresponding to change and deformation, and all these change and deformation should all belong to the protection domain of the claims in the present invention
Within.
Claims (10)
1. a kind of flame retarding polyether composition, it is characterised in that including following component in parts by weight：
2. flame retarding polyether composition as claimed in claim 1, it is characterised in that first PPG is according to following step
Suddenly it is prepared from：
1) first by melamine polyols and dimethylamine according to mol ratio 10：10-50min is stirred under 1 mixing, normal temperature condition, is obtained
To the first mixture；
2) phosphate and the second catalyst are added into first mixture, stirs, temperature is then increased to 80-
120 DEG C, reacted, the reaction time is 1.5-2.5h；The mass ratio of first mixture and the phosphate is 70:30；
Second catalyst is monoethanolamine manganate, and its consumption is the 1% of the phosphate quality；
3) temperature of question response system drops to less than 50 DEG C, vacuumizes, then heats up under conditions of the MPa of (- 0.02)-(- 0.1)
To 90-130 DEG C, continue to vacuumize, remove residual monomer, obtain first PPG.
3. flame retarding polyether composition as claimed in claim 2, it is characterised in that in step 3) in, the residual monomer of removing with
The mol ratio of first PPG is 1.8:100；Pressure is -0.1MPa when vacuumizing, and the time vacuumized is 2-3h.
4. flame retarding polyether composition as claimed in claim 1, it is characterised in that second PPG is according to following step
Suddenly it is prepared from：
1) first by isocyanuric acid polyalcohol and dimethylamine according to mol ratio 11.6：10-50min is stirred under 1 mixing, normal temperature condition,
Obtain the second mixture；
2) phosphate and the 3rd catalyst are added into second mixture, stirs, temperature is then increased to 80-
120 DEG C, reacted, the reaction time is 1.5-2.5h；The mass ratio of second mixture and the phosphate is 70:30；
3rd catalyst is monoethanolamine manganate, and its consumption is the 1% of the phosphate quality；
3) question response system temperature drops to less than 50 DEG C, vacuumizes, is then warming up under conditions of the MPa of (- 0.02)-(- 0.1)
90-130 DEG C, continue to vacuumize, remove residual monomer, obtain second PPG.
5. flame retarding polyether composition as claimed in claim 4, it is characterised in that in step 3) in, the residual monomer of removing with
The mol ratio 2.69 of second PPG:100；Pressure is -0.1MPa when vacuumizing, and the time vacuumized is 2-3h.
6. flame retarding polyether composition as claimed in claim 1, it is characterised in that
The viscosity of first PPG is 250-350, and hydroxyl value is 100-200；
The viscosity of second PPG is 9800-10200, and hydroxyl value is 100-200；
Average grain diameter≤2 μm of the silicate powder；
The stabilizer is the surfactant containing element silicon；
First catalyst is composite catalyst, and the composite catalyst is N, N', N "-three (dimethylamino-propyl)-hexahydro
Change any combination of triazine, (dimethylamino methyl) phenol of 2,4,6- tri- and pentamethyl-diethylenetriamine.
7. flame retarding polyether composition as claimed in claim 1, it is characterised in that including following component in parts by weight：
8. a kind of preparation method of flame retarding polyether composition as described in claim 1-7 any one, it is characterised in that according to
Following steps are prepared from：The PPG of formula ratio first is added in band high speed disperser reactor, with 60-80r/min
Speed stirring 10-20min；Then the stabilizer, water and the first catalyst of formula ratio are sequentially added, 15- is followed by stirring for
25min；The second PPG of formula ratio is subsequently added, continues to stir after 12-18min, adds the silicate powder of formula ratio,
70-80 DEG C is warming up to, 25-35min is stirred with 600-1000r/min speed, produced.
9. a kind of fire proofing, it is characterised in that as the flame retarding polyether composition described in claim 1-7 any one, and
Isocyanates is prepared from；The weight ratio of the flame retarding polyether composition and the isocyanates is 1：(1.3-1.5).
10. a kind of preparation method of fire proofing as claimed in claim 9, it is characterised in that according to following steps preparation
Into：The flame retarding polyether composition and the isocyanates are mixed, after stirring, in injection mould, compression molding.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112538147A (en) * | 2020-12-03 | 2021-03-23 | 广东金柏新材料科技股份有限公司 | Flame-retardant thermoplastic polyurethane material and preparation method thereof |
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Application publication date: 20170908 |