CN109880174A - A kind of preparation method of microencapsulation hypo-aluminum orthophosphate combustion inhibitor - Google Patents
A kind of preparation method of microencapsulation hypo-aluminum orthophosphate combustion inhibitor Download PDFInfo
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- CN109880174A CN109880174A CN201910225209.0A CN201910225209A CN109880174A CN 109880174 A CN109880174 A CN 109880174A CN 201910225209 A CN201910225209 A CN 201910225209A CN 109880174 A CN109880174 A CN 109880174A
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- hypo
- chlorinated paraffin
- aluminum orthophosphate
- ether
- microencapsulation
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 67
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 61
- 238000002485 combustion reaction Methods 0.000 title claims abstract description 26
- 239000003112 inhibitor Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 102
- 239000012188 paraffin wax Substances 0.000 claims abstract description 61
- 239000003063 flame retardant Substances 0.000 claims abstract description 38
- 238000000034 method Methods 0.000 claims abstract description 11
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 5
- 238000002390 rotary evaporation Methods 0.000 claims abstract description 4
- 229910052801 chlorine Inorganic materials 0.000 claims abstract 3
- 239000000843 powder Substances 0.000 claims description 20
- 238000005253 cladding Methods 0.000 claims description 13
- 239000004411 aluminium Substances 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000011574 phosphorus Substances 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001704 evaporation Methods 0.000 claims description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims 1
- 239000000460 chlorine Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 claims 1
- 239000001993 wax Substances 0.000 claims 1
- 229920006305 unsaturated polyester Polymers 0.000 abstract description 33
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 6
- 230000000979 retarding effect Effects 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000011159 matrix material Substances 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract 1
- 230000003000 nontoxic effect Effects 0.000 abstract 1
- 230000001681 protective effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 238000004321 preservation Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 150000003254 radicals Chemical class 0.000 description 4
- 229920006337 unsaturated polyester resin Polymers 0.000 description 4
- 239000004342 Benzoyl peroxide Substances 0.000 description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 3
- 235000019400 benzoyl peroxide Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000003094 microcapsule Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 125000002485 formyl group Chemical group [H]C(*)=O 0.000 description 1
- 239000002737 fuel gas Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- -1 phosphorus compound Chemical class 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000012306 spectroscopic technique Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Fireproofing Substances (AREA)
- Manufacturing Of Micro-Capsules (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of preparation methods of microencapsulation hypo-aluminum orthophosphate combustion inhibitor, the fire retardant is by the way that chlorinated paraffin to be dissolved into ether, hypo-aluminum orthophosphate is added in chlorinated paraffin diethyl ether solution again, pass through the ether in rotary evaporation removal system, to realize that the package to hypo-aluminum orthophosphate is handled, and by optimizing to raw material proportioning, the microencapsulation hypo-aluminum orthophosphate combustion inhibitor containing ignition-proof elements such as Al, P, Cl is obtained.Fire retardant of the present invention is applied to unsaturated polyester (UP), can effectively improve the compatibility and thermal stability of the fire retardant and matrix, improve the flame retardant property of unsaturated polyester (UP).Fire retardant of the present invention contains the ignition-proof elements such as Al, P, Cl, has cooperative flame retardant effect between molecular structure, makes fire retardant flame retarding efficiency with higher.Process flow involved in the present invention is simple, and preparation efficiency is high, and raw material sources are wide, cheap and nontoxic, environmentally protective, has application prospect well.
Description
Technical field
The invention belongs to fire retardant preparation and field of high polymer material modification, and in particular to a kind of microencapsulation time phosphorus
Application of the preparation method and the fire retardant of sour aluminium fire retardant in unsaturated polyester (UP) (UPR) material.
Background technique
As production and the development of science and technology and a variety of materials use the promotion of standard, people are to polymer composite
Performance propose various new demands.Today's society, polymer composite with metal material, inorganic non-metallic material
Expect that status is identical, becomes one of science and technology, important materials in economic construction.But polymer composite itself has inflammable
The characteristics of, seriously threaten our safety of life and property.Currently, in market all there is flame retarding efficiency in most fire retardant
It is low, poor compatibility, destroy basis material mechanical property the disadvantages of.Therefore, low toxic and environment-friendly, economical and efficient and compatible with matrix are researched and developed
The preferable fire retardant of property has become our current development trends.
Hypo-aluminum orthophosphate is a kind of novel fire retardant, it has that thermal stability is good, flame retarding efficiency is high, water solubility is small and to gathering
Closing object mechanical performance influences the advantages that small, is widely used in unsaturated polyester (UP), epoxy resin, poly- ammonia as fire retardant
The materials such as ester, polyvinyl chloride.Hypo-aluminum orthophosphate is capable of forming glassy or stable foam blanket at high temperature, can completely cut off sky
Oxygen in gas prevents fuel gas from escaping outward, to achieve the purpose that fire-retardant.In addition, containing in hypo-aluminum orthophosphate molecular structure
There is active P-H key, the fire retardation of free radical can be played during fire-retardant, it may have polymerization dehydration is catalyzed into carbon
Effect.The formation of polymer composites surface carbonation layer, on the one hand can prevent polymer from further decomposing, on the other hand can
The thermal decomposition generation for preventing it internal enters gas phase and participates in combustion process.But hypo-aluminum orthophosphate exists when using and storing
Biggish security risk, hypo-aluminum orthophosphate can decompose and discharge hydrogen phosphide under high temperature, hydrogen phosphide in air can spontaneous combustion, extreme
In the case of even can with air formed explosive mixture.
Chlorinated paraffin has the characteristics that chemical stability is good, noninflammability, hypotoxicity, water-resistance, dielectricity are good, therefore wide
It is general to be applied to polyvinyl chloride resin and rubber.Chlorinated paraffin can release HCl by thermal decomposition under alkaline condition, with rich carbon macromolecule
Close the high activity HO that object burning generates-、O2-And H+Free radical capture reaction occurs, generates inactive Cl-, it is suppressed that gas phase
Free radical chain reactions in burning, to obtain the fire-retardant effect of gas phase.In addition, chlorinated paraffin also will form solid matter isolation
Heat source, heat radiation, heat transfer.But flame retarding efficiency is lower when chlorinated paraffin is used alone, and higher additive amount can be to polymerization
The mechanical property loss of object basis material is larger.
Unsaturated polyester resin is one of maximum kind of development of thermosetting resins usage amount, and domestic glass reinforced plastic, people
Make the most matrix resin of the dosages such as stone, craftwork.But the molecular structure of unsaturated polyester resin determine its with it is most of
Polymer material is the same, has very high inflammability, limit oxygen index is only 19wt%.It is compound to study unsaturated polyester resin
The flame retardant property of material develops the unsaturated polyester resin kind with flame retardant property, expands it in all fields of national economy
Application be of great significance.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of microencapsulation hypo-aluminum orthophosphate combustion inhibitor, to realize to unsaturation
Polyester highly effective flame-retardant is modified.This method is adaptable by force, simple process, easy to operate, reaction condition is mild, flame retarding efficiency is high
Effect.
The purpose of the present invention is what is be achieved through the following technical solutions, a kind of preparation of microencapsulation hypo-aluminum orthophosphate combustion inhibitor
Method carries out package modification to hypo-aluminum orthophosphate using the chlorinated paraffin for being dissolved in diethyl ether solution under agitation, completes modified
Afterwards, through rotary evaporation, dry and remove ether after obtain microencapsulation hypo-aluminum orthophosphate combustion inhibitor, and using its to unsaturated polyester (UP) into
Row is flame-retardant modified, specifically include the following steps:
(1) chlorinated paraffin is dissolved in ether by mass volume ratio 1: 10g/mL~1: 30g/mL, obtains chlorinated paraffin second
Ethereal solution；
(2) by hypo-aluminum orthophosphate and chlorinated paraffin mass ratio 0.2~5.0, hypo-aluminum orthophosphate powder is added to obtained by step (1)
Chlorinated paraffin diethyl ether solution in, and the rotary evaporation 30min at 25 DEG C~30 DEG C removes ether, obtains chlorinated paraffin cladding
Hypo-aluminum orthophosphate powder；
(3) the resulting chlorinated paraffin cladding hypo-aluminum orthophosphate powder of step (2) is put in 40 DEG C of air dry oven dry
To ether evaporating completely, dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder is obtained；
(4) the resulting chlorinated paraffin cladding hypo-aluminum orthophosphate powder mull of step (3) is crossed into 200 meshes up to microencapsulation
Aluminum phosphate fire retardant.
In the present invention, the partial size of the hypo-aluminum orthophosphate is between 1-10 μm.
In the present invention, the chlorinated paraffin includes but is not limited to chlorinated paraffin 42, chlorinated paraffin 52, in chlorinated paraffin 70
One or more mixtures.
Due to the implementation of above technical scheme, the invention has the following advantages over the prior art:
1, cheap since fire retardant raw material sources provided by the present invention are extensive, and preparation process is simple, condition temperature
With, low energy consumption, and it is easy to operate, it is suitble to large-scale industrial production to use.
2, since in fire retardant provided by the invention, hypo-aluminum orthophosphate carries out cladding to it as carrier, by chlorinated paraffin
Reason, therefore the compatibility of hypo-aluminum orthophosphate and high polymer and the thermal stability of hypo-aluminum orthophosphate can be substantially improved.
3, since in fire retardant provided by the invention, hypo-aluminum orthophosphate and chlorinated paraffin produce good cooperative flame retardant and imitate
It answers, improves Char Residues Structure, therefore significantly improve the flame retardant property of the fire retardant.
4, fire retardant provided by the invention, hypo-aluminum orthophosphate decomposes at high temperature can generate the toxic combustible gas such as hydrogen phosphide,
The addition of chlorinated paraffin can both reduce the usage amount of hypo-aluminum orthophosphate, while the HCl of its release can capture free radical OH, to reach
To the effect for inhibiting burning.
5, fire retardant provided by the invention forms microcapsules since chlorinated paraffin is coated on hypo-aluminum orthophosphate surface, can
With enhance fire-retardant engineering material mechanical property and it is possible to prevente effectively from phosphorus compound introducing and cause material mechanical performance weak
The problem of change.
Detailed description of the invention
Fig. 1 is that the Fourier of microencapsulation hypo-aluminum orthophosphate combustion inhibitor prepared by the embodiment of the present invention 1,2,3,4,5 is infrared
Line spectrum (FTIR)；
Fig. 2 is the x-ray photoelectron of microencapsulation hypo-aluminum orthophosphate combustion inhibitor prepared by the embodiment of the present invention 1,2,3,4,5
Spectroscopic technique (XPS) analysis；
Fig. 3 is that the scanning electron microscope of hypo-aluminum orthophosphate used in the present invention shines (SEM)；
Fig. 4 is the electron scanning micrograph of microencapsulation hypo-aluminum orthophosphate combustion inhibitor prepared by present example 4；
Microencapsulation hypo-aluminum orthophosphate combustion inhibitor prepared by Fig. 5 embodiment of the present invention 1,2,3,4,5 is in a nitrogen atmosphere
Practical thermogravimetric curve (TAG)；
Fig. 6 is the flow chart that the present invention prepares microencapsulation hypo-aluminum orthophosphate combustion inhibitor；
Specific embodiment
The present invention is done below with reference to specific embodiment and more comprehensively, is meticulously described, but protection scope of the present invention is simultaneously
It is not limited to embodiment in detail below.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art
It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, is not intended to the limitation present invention
Protection scope.
Except there is a special instruction, the various reagents used in the present invention, raw material be can commodity commercially or
Person can the product as made from well known method.
With reference to the accompanying drawings and examples, the technical solution used to invention is further elaborated.
Embodiment 1
200ml ether is added in flask, the chlorinated paraffin of 25g is added, is stirred with glass bar, so that chlorinated paraffin is abundant
It is dissolved into formation chlorinated paraffin diethyl ether solution in ether.The hypo-aluminum orthophosphate of 5g is added in chlorinated paraffin diethyl ether solution, solution
Temperature is controlled at 25 DEG C, removes most ether in solution using Rotary Evaporators, then is placed on 40 DEG C of vacuum baking
In case, until powder is completely dried, remaining ether is removed, obtains dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder, then
Ground 200 mesh, obtains microencapsulation hypo-aluminum orthophosphate combustion inhibitor.
Embodiment 2
200ml ether is added in flask, the chlorinated paraffin of 20g is added, is stirred with glass bar, so that chlorinated paraffin is abundant
It is dissolved into formation chlorinated paraffin diethyl ether solution in ether.The hypo-aluminum orthophosphate of 10g is added in chlorinated paraffin diethyl ether solution, solution
Temperature is controlled at 25 DEG C, removes most ether in solution using Rotary Evaporators, then is placed on 40 DEG C of vacuum baking
In case, until powder is completely dried, remaining ether is removed, obtains dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder, then
Ground 200 mesh, obtains microencapsulation hypo-aluminum orthophosphate combustion inhibitor.
Embodiment 3
200ml ether is added in flask, the chlorinated paraffin of 15g is added, is stirred with glass bar, so that chlorinated paraffin is abundant
It is dissolved into formation chlorinated paraffin diethyl ether solution in ether.The hypo-aluminum orthophosphate of 15g is added in chlorinated paraffin diethyl ether solution, solution
Temperature is controlled at 25 DEG C, removes most ether in solution using Rotary Evaporators, then is placed on 40 DEG C of vacuum baking
In case, until powder is completely dried, remaining ether is removed, obtains dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder, then
Ground 200 mesh, obtains microencapsulation hypo-aluminum orthophosphate combustion inhibitor.
Embodiment 4
200ml ether is added in flask, the chlorinated paraffin of 10g is added, is stirred with glass bar, so that chlorinated paraffin is abundant
It is dissolved into formation chlorinated paraffin diethyl ether solution in ether.The hypo-aluminum orthophosphate of 20g is added in chlorinated paraffin diethyl ether solution, solution
Temperature is controlled at 25 DEG C, removes most ether in solution using Rotary Evaporators, then is placed on 40 DEG C of vacuum baking
In case, until powder is completely dried, remaining ether is removed, obtains dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder, then
Ground 200 mesh, obtains microencapsulation hypo-aluminum orthophosphate combustion inhibitor.
Embodiment 5
200ml ether is added in flask, the chlorinated paraffin of 5g is added, is stirred with glass bar, so that chlorinated paraffin is abundant
It is dissolved into formation chlorinated paraffin diethyl ether solution in ether.The hypo-aluminum orthophosphate of 25g is added in chlorinated paraffin diethyl ether solution, solution
Temperature is controlled at 25 DEG C, removes most ether in solution using Rotary Evaporators, then is placed on 40 DEG C of vacuum baking
In case, until powder is completely dried, remaining ether is removed, obtains dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder, then
Ground 200 mesh, obtains microencapsulation hypo-aluminum orthophosphate combustion inhibitor.
Embodiment 6
The preparation of pure unsaturated polyester (UP)
Pure unsaturated polyester (UP) is control group, weighs 100g unsaturated polyester (UP) (191#), the initiator benzoyl peroxide of 2g is added
Formyl pours into mold after mechanical stirring is uniform, in 80 DEG C of heat preservations 1h, 110 DEG C of heat preservation 3h.Then demoulding sampling.
Prepared flame retardant type unsaturated polyester (UP), which is tested its oxygen index (OI) according to GB/T 2406.2-2009 method, is
19.8%.
Prepared flame retardant type unsaturated polyester (UP), which is tested its vertical combustion level results according to GB/T 2408-2008, is
Off grade.
Embodiment 7
Hypo-aluminum orthophosphate-chlorinated paraffin/unsaturated polyester composite preparation
The chlorinated paraffin of the hypo-aluminum orthophosphate of the unsaturated polyester (UP) of 70g and 20g, 10g are mixed, added after mechanical stirring 30min
The initiator benzoyl peroxide for entering 1.4g, pours into mold after mixing evenly, in 80 DEG C of heat preservations 1h, 110 DEG C of heat preservation 3h.Then it takes off
Mould sampling.
Prepared flame retardant type unsaturated polyester (UP), which is tested its oxygen index (OI) according to GB/T 2406.2-2009 method, is
27.5%.
Prepared flame retardant type unsaturated polyester (UP), which is tested its vertical combustion level results according to GB/T 2408-2008, is
V-2 grades.
Embodiment 8
The application of microencapsulation hypo-aluminum orthophosphate combustion inhibitor
The preparation of microencapsulation hypo-aluminum orthophosphate combustion inhibitor is with embodiment 4, by the microcapsules of the unsaturated polyester (UP) of 70g and 30g
Change hypo-aluminum orthophosphate combustion inhibitor mixing, the initiator benzoyl peroxide of 1.4g is added after mechanical stirring 30min, falls after mixing evenly
Enter mold, in 80 DEG C of heat preservations 1h, 110 DEG C of heat preservation 3h.Then demoulding sampling.
Prepared flame retardant type unsaturated polyester (UP), which is tested its oxygen index (OI) according to GB/T 2406.2-2009 method, is
28.5%.
Prepared flame retardant type unsaturated polyester (UP), which is tested its vertical combustion level results according to GB/T 2408-2008, is
V-0 grades.
The present invention is described in detail above, its object is to allow the personage for being familiar with this field technology that can understand this
The content of invention is simultaneously implemented, and it is not intended to limit the scope of the present invention, all Spirit Essence institutes according to the present invention
The equivalent change or modification of work should be all included within the scope of protection of the present invention.
Claims (3)
1. a kind of preparation method of microencapsulation hypo-aluminum orthophosphate combustion inhibitor, which comprises the following steps:
(1) chlorinated paraffin is dissolved in ether by mass volume ratio 1: 10g/mL~1: 30g/mL, it is molten obtains chlorinated paraffin ether
Liquid；
(2) by hypo-aluminum orthophosphate and chlorinated paraffin mass ratio 0.2~5.0, hypo-aluminum orthophosphate powder is added to step (1) resulting chlorine
In fossil waxes diethyl ether solution, and the rotary evaporation 30min at 25 DEG C~30 DEG C, ether is removed, chlorinated paraffin is obtained and coats time phosphorus
Sour aluminium powder；
(3) the resulting chlorinated paraffin cladding hypo-aluminum orthophosphate powder of step (2) is put in 40 DEG C of air dry oven and is dried to second
Ether evaporating completely obtains dry chlorinated paraffin cladding hypo-aluminum orthophosphate powder；
(4) the resulting chlorinated paraffin cladding hypo-aluminum orthophosphate powder mull of step (3) is crossed into 200 meshes up to microencapsulation hypophosphorous acid
Aluminium fire retardant.
2. according to the method described in claim 1, it is characterized by: the partial size of hypo-aluminum orthophosphate is between 1-10 μm.
3. according to the method described in claim 1, it is characterized by: the chlorinated paraffin include but is not limited to chlorinated paraffin 42,
One of chlorinated paraffin 52, chlorinated paraffin 70 or a variety of mixtures.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110615936A (en) * | 2019-10-09 | 2019-12-27 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying styrene resin and preparation method thereof |
| CN111961254A (en) * | 2020-08-27 | 2020-11-20 | 湖北航天化学技术研究所 | Preparation method of modified aluminum hypophosphite flame retardant |
| CN114085422A (en) * | 2021-11-30 | 2022-02-25 | 广东宇星阻燃新材股份有限公司 | Preparation method of inorganic aluminum hypophosphite and application of inorganic aluminum hypophosphite in flame-retardant PBT |
| CN114958014A (en) * | 2019-08-05 | 2022-08-30 | 航天特种材料及工艺技术研究所 | Composition, efficient flame-retardant phase-change heat management composite material prepared from composition and preparation method of composite material |
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| CN101885859A (en) * | 2009-05-11 | 2010-11-17 | 中国科学院化学研究所 | Flame retardant microcapsule and application thereof |
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| CN110615936A (en) * | 2019-10-09 | 2019-12-27 | 江苏万纳普新材料科技有限公司 | Special halogen-free flame-retardant synergistic functional master batch for modifying styrene resin and preparation method thereof |
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| CN111961254A (en) * | 2020-08-27 | 2020-11-20 | 湖北航天化学技术研究所 | Preparation method of modified aluminum hypophosphite flame retardant |
| CN114085422A (en) * | 2021-11-30 | 2022-02-25 | 广东宇星阻燃新材股份有限公司 | Preparation method of inorganic aluminum hypophosphite and application of inorganic aluminum hypophosphite in flame-retardant PBT |
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