CN104592301A - Flame retardant, preparation method as well as modified polydicyclopentadiene and preparation method - Google Patents
Flame retardant, preparation method as well as modified polydicyclopentadiene and preparation method Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 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 title abstract description 24
- 229920001153 Polydicyclopentadiene Polymers 0.000 title abstract description 12
- HECLRDQVFMWTQS-RGOKHQFPSA-N 1755-01-7 Chemical compound C1[C@H]2[C@@H]3CC=C[C@@H]3[C@@H]1C=C2 HECLRDQVFMWTQS-RGOKHQFPSA-N 0.000 claims abstract description 40
- -1 methoxyl cyclotriphosphazene pentachloride Chemical compound 0.000 claims abstract description 19
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000012986 modification Methods 0.000 claims description 28
- 230000004048 modification Effects 0.000 claims description 28
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Natural products OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 26
- 239000002131 composite material Substances 0.000 claims description 25
- 239000003054 catalyst Substances 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010792 warming Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000011261 inert gas Substances 0.000 claims description 3
- 239000012044 organic layer Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 238000010107 reaction injection moulding Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- UUUXFTDKVRVJJC-UHFFFAOYSA-N phenol;tungsten Chemical compound [W].OC1=CC=CC=C1 UUUXFTDKVRVJJC-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 13
- 238000000034 method Methods 0.000 abstract description 3
- NSTVHFOHEYKXRQ-UHFFFAOYSA-N 4-bicyclo[2.2.1]hept-2-enylmethanol Chemical group C1CC2C=CC1(CO)C2 NSTVHFOHEYKXRQ-UHFFFAOYSA-N 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 17
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 16
- 239000011259 mixed solution Substances 0.000 description 10
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- WQDUMFSSJAZKTM-UHFFFAOYSA-N Sodium methoxide Chemical group [Na+].[O-]C WQDUMFSSJAZKTM-UHFFFAOYSA-N 0.000 description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000001746 injection moulding Methods 0.000 description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 5
- 125000005574 norbornylene group Chemical group 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 description 4
- 235000011152 sodium sulphate Nutrition 0.000 description 4
- 238000000465 moulding Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 239000004411 aluminium Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- HQMRIBYCTLBDAK-UHFFFAOYSA-M bis(2-methylpropyl)alumanylium;chloride Chemical compound CC(C)C[Al](Cl)CC(C)C HQMRIBYCTLBDAK-UHFFFAOYSA-M 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- YZCKVEUIGOORGS-IGMARMGPSA-N Protium Chemical compound [1H] YZCKVEUIGOORGS-IGMARMGPSA-N 0.000 description 1
- 241000720974 Protium Species 0.000 description 1
- LDBRVTIIJPNARY-UHFFFAOYSA-N [W].C(CCC)C1=C(C=CC=C1)O Chemical compound [W].C(CCC)C1=C(C=CC=C1)O LDBRVTIIJPNARY-UHFFFAOYSA-N 0.000 description 1
- CYQHEBLFEAIVCG-UHFFFAOYSA-N [W].C(CCCCC)C1=C(C=CC=C1)O Chemical compound [W].C(CCCCC)C1=C(C=CC=C1)O CYQHEBLFEAIVCG-UHFFFAOYSA-N 0.000 description 1
- AUUVJHTZAHJATM-UHFFFAOYSA-N [W].C(CCCCCCC)C1=C(C=CC=C1)O Chemical compound [W].C(CCCCCCC)C1=C(C=CC=C1)O AUUVJHTZAHJATM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000002274 desiccant Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
Landscapes
- Polyoxymethylene Polymers And Polymers With Carbon-To-Carbon Bonds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a flame retardant, a preparation method as well as modified polydicyclopentadiene and a preparation method and belongs to the technical field of flame retardant materials. According to the flame retardant disclosed by the invention, by taking a phosphonitrilic chloride trimer as a matrix which is connected with a norbornene methanol group, the flame retardant has a good co-dissolving and co-polymerizing characteristic with dicyclopentadiene for modifying dicyclopentadiene. The invention discloses the flame retardant modified polydicyclopentadiene material which is blended and polymerized by dicyclopentadiene and the flame retardant, wherein the flame retardant is 3-15% by mass of dicyclopentadiene. By using mono-norborneol methoxyl cyclotriphosphazene pentachloride as the flame retardant, compared with a pure polydicyclopentadiene material, a few flame retardant is added to obviously improve the flame retardant performance of polydicyclopentadiene and meanwhile, the mechanical property is not reduced. The preparation method disclosed by the invention is simple in craft process, easy to control and realize, and suitable for industrialized popularization and application.
Description
Technical field
The invention belongs to fire retardant material technical field, be specifically related to fire retardant, preparation method and modification Polydicyclopentadiencomposite composite material, preparation method.
Background technology
Polydicyclopentadiene is a kind of novel hot setting engineering plastics, there is excellent comprehensive mechanical property, as good strength and toughness balance, good dimensional stability, resistance to acids and bases, excellent application and electrical insulation capability etc., therefore, Application Areas is very extensive.But, only containing carbon, protium in dicyclopentadiene material, belong to inflammable material, which has limited its application in some special dimension.For this reason, people overcome this deficiency by the method for adding various fire retardant, but, the catalyst system of dicyclopentadiene ring-opening polymerization has higher susceptibility to a lot of fire retardant, general fire retardant easily makes catalyst system inactivation, therefore, when using fire retardant modification dicyclopentadiene, suitable fire retardant must be selected.
Hexachlorocyclotriphosphazene is a kind of compound simultaneously containing chlorine, nitrogen, phosphoric, self can form a fire-retardant collaboration system, thus there is good flame retardant properties, but hexachlorocyclotriphosphazene nature is comparatively active, and be insoluble to dicyclopentadiene, therefore, have to pass through modified could as the fire retardant of modification polydicyclopentadiene.
Summary of the invention
An object of the present invention be to provide a kind of can with the polymerizability phosphonitrile fire retardant of dicyclopentadiene copolymerization, solve existing fire retardant and be insoluble to dicyclopentadiene monomer and the problem affecting reaction injection moulding, realize the fire-retardant object of polydicyclopentadiene.
Second object of the present invention is to provide a kind of preparation method of fire retardant;
3rd object of the present invention is to provide a kind of Polydicyclopentadiencomposite composite material of fire retardant modification;
Meanwhile, the present invention is also the preparation method of the Polydicyclopentadiencomposite composite material providing a kind of fire retardant modification.
To achieve these goals, the technical solution used in the present invention is:
A kind of fire retardant, its structural formula is:
be single norbornylene ylmethoxy pentachloro-ring three phosphonitrile.
The preparation method of above-mentioned fire retardant, comprises following operation steps:
1) under protection of inert gas, add in organic solvent by the norbornylene methyl alcohol and sodium alkoxide that wait amount of substance, reaction, obtains mixture;
2) to step 1) add the hexachlorocyclotriphosphazene with the amount of substance such as norbornylene methyl alcohol in gained mixture, after reaction, washing in, extract to obtain organic layer, after drying, namely obtain described fire retardant.
Described sodium alkoxide is sodium methylate.
Described organic solvent is tetrahydrofuran (THF).
Step 1) described in reaction be stirring reaction 1 ~ 4 hour at 70 ~ 90 DEG C.
In step 2, by step 1) after gained mixture is cooled to room temperature, add the hexachlorocyclotriphosphazene with amount of substances such as norbornylene methyl alcohol.
Step 2) described in react for being warming up to 80 ~ 100 DEG C, react 3 ~ 6 hours.
Step 2) described in dry for by anhydrous sodium sulphate as desiccant dryness organic layer.
Adopt a modification Polydicyclopentadiencomposite composite material for above-mentioned fire retardant, formed by dicyclopentadiene and fire retardant blending polymerization, the quality of fire retardant is 3% ~ 15% of dicyclopentadiene quality.
The preparation method of above-mentioned modification Polydicyclopentadiencomposite composite material is, after being mixed by described fire retardant, by reaction injection moulding, obtains described modification Polydicyclopentadiencomposite composite material with dicyclopentadiene, Primary Catalysts, promotor.
Described Primary Catalysts is 1:1000 ~ 2000 with the amount of substance ratio of dicyclopentadiene; Described promotor is 20 ~ 50:1 with the amount of substance ratio of Primary Catalysts.
Described Primary Catalysts is tungsten phenol complex compound, and its general structure is W (OPhR)
3cl
3; Wherein OPhR is alkyl phenoxy, R to be carbonatoms be 4 ~ 9 alkyl, R can replace arbitrarily position and replace on phenyl ring.
The concrete structure of described alkyl phenoxy is as follows:
Described promotor is aluminum alkyls.
Described aluminum alkyls is a chloro-di-isobutyl aluminum, triisobutyl aluminium or aluminium diethyl monochloride.
The preparation method of above-mentioned modification Polydicyclopentadiencomposite composite material, comprises following operation steps:
1) under protection of inert gas, fire retardant is dissolved in liquid dicyclopentadiene, obtains mixed solution;
2) mixed solution is divided into two portions, in a part of mixed solution, adds the Primary Catalysts of dicyclopentadiene total mole number 1/1000 ~ 1/2000, obtain solution A; In another part mixed solution, add the promotor of described aryloxy tungsten catalyst mole number 20 ~ 50 times, obtain solution B;
3) by solution A and solution B hybrid injection shaping, obtain modification Polydicyclopentadiencomposite composite material.
Described rare gas element is nitrogen.
The reaction equation that the present invention prepares fire retardant is:
Fire retardant of the present invention, take hexachlorocyclotriphosphazene as parent, with the group of norbornylene methyl alcohol structure in connection, form the compound simultaneously containing chlorine, nitrogen, phosphorus, self can form a cooperative flame retardant system, there is good flame retardant properties, simultaneously, the norbornylene group that it connects makes itself and dicyclopentadiene have good consistency, can carry out copolyreaction, obtain the Polydicyclopentadiencomposite composite material with good flame-retardance with dicyclopentadiene monomer.
Fire retardant modification Polydicyclopentadiencomposite composite material of the present invention, selects norcamphyl methoxyl group pentachloro-ring three phosphonitrile as fire retardant, only needs to add fire retardant on a small quantity, can improve the flame retardant properties of polydicyclopentadiene significantly, do not reduce its mechanical property simultaneously.
Preparation method's technological process of the present invention is simple, is easy to control and realize, and is suitable for industrial application.
Embodiment
Below in conjunction with specific embodiment, fire retardant modification Polydicyclopentadiencomposite composite material of the present invention is described in detail, but does not limit technical scheme of the present invention.The raw material dicyclopentadiene related in embodiment is commercially available prod, and content is greater than 98%; Hexachlorocyclotriphosphazene is commercially available prod, and content is greater than 99%; Norbornylene methyl alcohol is commercially available prod, and content is greater than 99%.
Embodiment 1
The present embodiment fire retardant chemical structural formula is:
The preparation method of the present embodiment fire retardant, concrete operation step is as follows: under nitrogen protection, in 200mL tetrahydrofuran (THF), norbornylene methyl alcohol and the sodium methylate of amount such as to add, at 70 DEG C, stirring reaction is after 1 hour, after reaction system is cooled to room temperature, add the hexachlorocyclotriphosphazene with amounts such as norbornylene methyl alcohol, then 100 DEG C are warming up to, react after 3 hours, be cooled to room temperature, add water washing to neutral, filter after organic over anhydrous dried over sodium sulfate, steam solvent, product is single norbornylene ylmethoxy pentachloro-ring three phosphonitrile, content is 84%.
The fire retardant modification Polydicyclopentadiencomposite composite material of the present embodiment is formed by dicyclopentadiene and fire retardant blending polymerization, and the quality of fire retardant is 3% of dicyclopentadiene quality.
The preparation of the present embodiment flame-retardant modified polydicyclopentadiene, concrete operation step is as follows:
1) under nitrogen protection, 6 parts by weight of flame retardant are dissolved in the liquid dicyclopentadiene of 200 weight parts, obtains mixed solution;
2) mixed solution is added in A, B storage tank of injection moulding machine; Add Primary Catalysts butylphenol tungsten complex at A storage tank, the mol ratio of Primary Catalysts and the total consumption of dicyclopentadiene is 1:1000; In B storage tank, add promotor one chloro-di-isobutyl aluminum, the mol ratio of promotor and Primary Catalysts is 20:1;
3) open reactor injection moulding machine, the feed liquid in A, B storage tank injects die for molding after mixing tank mixing, obtains fire retardant modification Polydicyclopentadiencomposite composite material.
Embodiment 2
The present embodiment fire retardant chemical structural formula is:
The preparation method of the present embodiment fire retardant is, concrete operation step is as follows: under nitrogen protection, in 200ml tetrahydrofuran (THF), norbornylene methyl alcohol and the sodium methylate of amount such as to add, at 80 DEG C, stirring reaction is after 2 hours, after reaction system is cooled to room temperature, add the hexachlorocyclotriphosphazene with amounts such as norbornylene methyl alcohol, then 90 DEG C are warming up to, react after 5 hours, be cooled to room temperature, add water washing to neutral, filter after organic over anhydrous dried over sodium sulfate, steam solvent, product is single norbornylene ylmethoxy pentachloro-ring three phosphonitrile, content is 90.5%.
The present embodiment fire retardant modification Polydicyclopentadiencomposite composite material is formed by dicyclopentadiene and fire retardant blending polymerization, and the quality of fire retardant is 5% of dicyclopentadiene quality.
The preparation method of the present embodiment fire retardant modification polydicyclopentadiene is that concrete operation step is as follows:
1) under nitrogen protection, 10 parts by weight of flame retardant are dissolved in the liquid dicyclopentadiene of 200 weight parts, obtains mixed solution;
2) added by mixed solution in A, B storage tank of injection moulding machine, add Primary Catalysts hexyl phenol tungsten complex at A storage tank, the mol ratio of Primary Catalysts and the total consumption of dicyclopentadiene is 1:1500; In B storage tank, add promotor triisobutyl aluminium, the mol ratio of promotor and Primary Catalysts is 30:1;
3) open reactor injection moulding machine, the feed liquid in A, B storage tank injects die for molding after mixing tank mixing, obtains fire retardant modification Polydicyclopentadiencomposite composite material.
Embodiment 3
The present embodiment fire retardant chemical structural formula is:
The preparation method of the present embodiment fire retardant is, concrete operation steps is as follows: under nitrogen protection, in 200ml tetrahydrofuran (THF), norbornylene methyl alcohol and the sodium methylate of amount such as to add, at 90 DEG C, stirring reaction is after 4 hours, after reaction system is cooled to room temperature, add the hexachlorocyclotriphosphazene with amounts such as norbornylene methyl alcohol, then 80 DEG C are warming up to, react after 6 hours, be cooled to room temperature, add water washing to neutral, filter after organic over anhydrous dried over sodium sulfate, steam solvent, product is single norbornylene ylmethoxy pentachloro-ring three phosphonitrile, content is 93.5%.
The present embodiment fire retardant modification Polydicyclopentadiencomposite composite material is formed by dicyclopentadiene and fire retardant blending polymerization, and the quality of fire retardant is 15% of dicyclopentadiene quality.
The preparation method of the present embodiment fire retardant modification polydicyclopentadiene is that concrete operation step is as follows:
1) under nitrogen protection, 20 parts by weight of flame retardant are dissolved in the liquid dicyclopentadiene of 200 weight parts, obtains mixed solution;
2) added by mixed solution in A, B storage tank of injection moulding machine, add Primary Catalysts octyl phenol tungsten complex at A storage tank, the mol ratio of Primary Catalysts and the total consumption of dicyclopentadiene is 1:2000; In B storage tank, add promotor aluminium diethyl monochloride, the mol ratio of promotor and Primary Catalysts is 50:1;
3) open reactor injection moulding machine, the feed liquid in A, B storage tank injects die for molding after mixing tank mixing, obtains fire retardant modification Polydicyclopentadiencomposite composite material.
Comparative example
The dicyclopentadiene material of this comparative example in the preparation, does not comprise fire retardant in raw material, and all the other are with embodiment 1.
Contrast experiment
This experiment is tested the flame retardant properties of embodiment 1 ~ 3 and comparative example gained dicyclopentadiene material and impact property, and result is as shown in table 1
The flame retardant properties of table 1 embodiment 1-3 and comparative example obtained flame-retardant dicyclopentadiene material and impact property detected result
| Object | Oxygen index (%) | Shock strength (J/m) |
| Embodiment 1 | 20.1 | 289.7 |
| Embodiment 2 | 24.4 | 293.4 |
| Embodiment 3 | 28.7 | 288.3 |
| Comparative example | 19.3 | 285.2 |
As can be seen from Table 1, the shock strength of embodiment 1 ~ 3 obtained flame-retardant dicyclopentadiene material is all greater than comparative example, and oxygen index is also significantly improved.Test-results shows, relative to common dicyclopentadiene material, of the present inventionly employ reactable fire retardant modification Polydicyclopentadiencomposite composite material, by controlling the interpolation consumption of fire retardant, do not reducing on the basis of material mechanical performance, greatly improving the flame retardant properties of material.
Claims (10)
1. a fire retardant, is characterized in that, its structural formula is:
2. a preparation method for fire retardant as claimed in claim 1, is characterized in that, comprises following operation steps:
1) under protection of inert gas, add in organic solvent by the norbornylene methyl alcohol and sodium alkoxide that wait amount of substance, reaction, obtains mixture;
2) to step 1) add the hexachlorocyclotriphosphazene with the amount of substance such as norbornylene methyl alcohol in gained mixture, after reaction, washing, to neutral, extract to obtain organic layer, namely obtains described fire retardant after drying.
3. the preparation method of fire retardant as claimed in claim 2, is characterized in that, step 1) described in reaction be stirring reaction 1 ~ 4 hour at 70 ~ 90 DEG C.
4. the preparation method of fire retardant as claimed in claim 2, is characterized in that, in step 2, by step 1) after gained mixture is cooled to room temperature, add the hexachlorocyclotriphosphazene with the amount of substance such as norbornylene methyl alcohol.
5. the preparation method of fire retardant as claimed in claim 2, is characterized in that, step 2) described in react for being warming up to 80 ~ 100 DEG C, react 3 ~ 6 hours.
6. adopt a modification Polydicyclopentadiencomposite composite material for fire retardant as claimed in claim 1, it is characterized in that, formed by dicyclopentadiene and fire retardant blending polymerization, the quality of fire retardant is 3% ~ 15% of dicyclopentadiene quality.
7. the preparation method of a modification Polydicyclopentadiencomposite composite material as claimed in claim 6, it is characterized in that, after being mixed with dicyclopentadiene, Primary Catalysts, promotor by described fire retardant, by reaction injection moulding, obtain described modification Polydicyclopentadiencomposite composite material.
8. the preparation method of modification Polydicyclopentadiencomposite composite material as claimed in claim 7, is characterized in that, described Primary Catalysts is 1:1000 ~ 2000 with the amount of substance ratio of dicyclopentadiene; Described promotor is 20 ~ 50:1 with the amount of substance ratio of Primary Catalysts.
9. the preparation method of modification Polydicyclopentadiencomposite composite material as claimed in claim 7, it is characterized in that, described Primary Catalysts is tungsten phenol complex compound, and its general structure is W (OPhR)
3cl
3; Wherein OPhR is alkyl phenoxy, R to be carbonatoms be 4 ~ 9 alkyl.
10. the preparation method of modification Polydicyclopentadiencomposite composite material as claimed in claim 7, it is characterized in that, described promotor is aluminum alkyls.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017071161A1 (en) * | 2015-10-28 | 2017-05-04 | 广东生益科技股份有限公司 | Cyclotriphosphazene halogen-free flame retardant containing imide structure, and preparation method and use |
| CN112552346A (en) * | 2020-12-25 | 2021-03-26 | 厦门产业技术研究院 | Hexachlorocyclotriphosphazene derivative, preparation method and application thereof, polydicyclopentadiene composite material and preparation method thereof |
| CN114790260A (en) * | 2022-04-02 | 2022-07-26 | 安徽建筑大学 | High-modulus, high-impact, wear-resistant and heat-resistant intrinsic flame-retardant polydicyclopentadiene engineering material and preparation method thereof |
| CN114804078A (en) * | 2022-03-18 | 2022-07-29 | 安徽建筑大学 | Polydicyclopentadiene-based carbon nanotube/graphene nanosheet aerogel flame-retardant electromagnetic shielding composite material and preparation method thereof |
| CN114835556A (en) * | 2022-05-11 | 2022-08-02 | 常州巨德新材料有限公司 | Bromine-containing norbornene derivative, preparation method thereof and flame-retardant polydicyclopentadiene material |
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| WO2017071161A1 (en) * | 2015-10-28 | 2017-05-04 | 广东生益科技股份有限公司 | Cyclotriphosphazene halogen-free flame retardant containing imide structure, and preparation method and use |
| CN106632487A (en) * | 2015-10-28 | 2017-05-10 | 广东生益科技股份有限公司 | Cyclotriphosphazene halogen-free flame retardant containing imide structure, preparation method and use thereof |
| CN106632487B (en) * | 2015-10-28 | 2018-12-25 | 广东生益科技股份有限公司 | Three phosphonitrile halogen-free flame retardants of ring, Preparation method and use containing imide structure |
| CN112552346A (en) * | 2020-12-25 | 2021-03-26 | 厦门产业技术研究院 | Hexachlorocyclotriphosphazene derivative, preparation method and application thereof, polydicyclopentadiene composite material and preparation method thereof |
| CN112552346B (en) * | 2020-12-25 | 2024-02-06 | 厦门产业技术研究院 | Hexachlorocyclotriphosphazene derivative, preparation method and application thereof, polydicyclopentadiene composite material and preparation method thereof |
| CN114804078A (en) * | 2022-03-18 | 2022-07-29 | 安徽建筑大学 | Polydicyclopentadiene-based carbon nanotube/graphene nanosheet aerogel flame-retardant electromagnetic shielding composite material and preparation method thereof |
| CN114804078B (en) * | 2022-03-18 | 2023-07-04 | 安徽建筑大学 | Poly-dicyclopentadienyl carbon nano tube/graphene nano sheet aerogel flame-retardant electromagnetic shielding composite material and preparation method thereof |
| CN114790260A (en) * | 2022-04-02 | 2022-07-26 | 安徽建筑大学 | High-modulus, high-impact, wear-resistant and heat-resistant intrinsic flame-retardant polydicyclopentadiene engineering material and preparation method thereof |
| CN114790260B (en) * | 2022-04-02 | 2023-04-18 | 安徽建筑大学 | High-modulus, high-impact, wear-resistant and heat-resistant intrinsic flame-retardant polydicyclopentadiene engineering material and preparation method thereof |
| CN114835556A (en) * | 2022-05-11 | 2022-08-02 | 常州巨德新材料有限公司 | Bromine-containing norbornene derivative, preparation method thereof and flame-retardant polydicyclopentadiene material |
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| CN104592301B (en) | 2016-08-17 |
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