CN104497354B - A kind of triguaiacyl phosphate polyhedral oligomeric sesquialter polysiloxanes fire retardant and preparation method thereof - Google Patents
A kind of triguaiacyl phosphate polyhedral oligomeric sesquialter polysiloxanes fire retardant and preparation method thereof Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 43
- -1 polysiloxanes Polymers 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 11
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 9
- 239000010452 phosphate Substances 0.000 title claims abstract description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 7
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims abstract description 14
- FCVNATXRSJMIDT-UHFFFAOYSA-N trihydroxy(phenyl)silane Chemical compound O[Si](O)(O)C1=CC=CC=C1 FCVNATXRSJMIDT-UHFFFAOYSA-N 0.000 claims abstract description 13
- HXBZCHYDLURWIZ-UHFFFAOYSA-N diphenyl hydrogen phosphate;hydrochloride Chemical compound Cl.C=1C=CC=CC=1OP(=O)(O)OC1=CC=CC=C1 HXBZCHYDLURWIZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000006482 condensation reaction Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004821 distillation Methods 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- XJWOWXZSFTXJEX-UHFFFAOYSA-N phenylsilicon Chemical compound [Si]C1=CC=CC=C1 XJWOWXZSFTXJEX-UHFFFAOYSA-N 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 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 10
- 229920000642 polymer Polymers 0.000 abstract description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 5
- 239000011574 phosphorus Substances 0.000 abstract description 5
- 229910052710 silicon Inorganic materials 0.000 abstract description 2
- 239000010703 silicon Substances 0.000 abstract description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract 1
- 238000009833 condensation Methods 0.000 abstract 1
- 230000005494 condensation Effects 0.000 abstract 1
- 235000010290 biphenyl Nutrition 0.000 description 19
- 239000004305 biphenyl Substances 0.000 description 19
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 19
- 239000000463 material Substances 0.000 description 6
- 235000021317 phosphate Nutrition 0.000 description 6
- 238000001228 spectrum Methods 0.000 description 5
- 229910008051 Si-OH Inorganic materials 0.000 description 4
- 229910006358 Si—OH Inorganic materials 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000019504 cigarettes Nutrition 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000005012 migration Effects 0.000 description 3
- 238000013508 migration Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229920000388 Polyphosphate Polymers 0.000 description 2
- 229910002808 Si–O–Si Inorganic materials 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- DWNAQMUDCDVSLT-UHFFFAOYSA-N diphenyl phthalate Chemical compound C=1C=CC=C(C(=O)OC=2C=CC=CC=2)C=1C(=O)OC1=CC=CC=C1 DWNAQMUDCDVSLT-UHFFFAOYSA-N 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000001205 polyphosphate Substances 0.000 description 2
- 235000011176 polyphosphates Nutrition 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- GUKSXDYMYSUAMN-UHFFFAOYSA-M C(C)C(COP(=O)(OCC(CCCC)CC)[O-])CCCC.[Cl+] Chemical compound C(C)C(COP(=O)(OCC(CCCC)CC)[O-])CCCC.[Cl+] GUKSXDYMYSUAMN-UHFFFAOYSA-M 0.000 description 1
- ASMQGLCHMVWBQR-UHFFFAOYSA-N Diphenyl phosphate Chemical class C=1C=CC=CC=1OP(=O)(O)OC1=CC=CC=C1 ASMQGLCHMVWBQR-UHFFFAOYSA-N 0.000 description 1
- PBVHFLNOPHXNNK-UHFFFAOYSA-N O=P(OC1C=CC=CC1)(Oc1ccccc1)Cl Chemical compound O=P(OC1C=CC=CC1)(Oc1ccccc1)Cl PBVHFLNOPHXNNK-UHFFFAOYSA-N 0.000 description 1
- 229910004852 P—O—Si Inorganic materials 0.000 description 1
- YSMRWXYRXBRSND-UHFFFAOYSA-N TOTP Chemical compound CC1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C)OC1=CC=CC=C1C YSMRWXYRXBRSND-UHFFFAOYSA-N 0.000 description 1
- WPGUUPJOAVPZBQ-UHFFFAOYSA-N [Cl].OP(O)(O)=O Chemical compound [Cl].OP(O)(O)=O WPGUUPJOAVPZBQ-UHFFFAOYSA-N 0.000 description 1
- GJMMXPXHXFHBPK-UHFFFAOYSA-N [P].[Cl] Chemical compound [P].[Cl] GJMMXPXHXFHBPK-UHFFFAOYSA-N 0.000 description 1
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000001195 anabolic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 150000004760 silicates Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Fireproofing Substances (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a kind of triguaiacyl phosphate polyhedral oligomeric sesquialter polysiloxanes fire retardant and preparation method thereof, the fire retardant has following structure：
Description
Technical field
It is to be related to a kind of triguaiacyl phosphate polyhedral oligomeric sesquialter to gather specifically the present invention relates to a kind of phosphorus silicon composite flame-retardant agent
Siloxane flame retardant and preparation method thereof, belongs to technical field of flame retardant.
Background technology
Phosphate ester flame retardants are the favorites of organic halogen-free agent, belong to the category of expansion type flame retardant, obtain in recent years
Obtained huge development.However, widely used phosplate based flame retardant, such as triphenyl phosphate, tricresyl phosphate in the market
Toluene ester etc., has that relative molecular weight is small, volatility is big, heat decomposition temperature is relatively low, easily occurs from material in use
The deficiency such as migration and volatilization loss in material, therefore, their application effect is not good.
Polyphosphate fire retardant is a class New-type halide-free, low cigarette, low toxicity, resistance to migration, resistance to volatilization, the resistance of radiation-resistant environment-friendly type
Agent is fired, with the features such as relative molecular mass is big, phosphorus content is high, flame retardant effect is lasting.Polyphosphoric acid in polyphosphate fire retardant
Phenyl ester also has plasticising performance concurrently, and its plasticity, anti-flammability, heat endurance are superior to common phosplate, however, it with it is other
Expansion type flame retardant is the same, and the compatibility with polymer substrate is poor.
Polyhedral oligomeric sesquialter polysiloxanes is the organic/inorganic nano-hybrid materials that a class is new, possess nanostructured,
Advantage with both polymer and inorganic material, shows good flame retardant effect.Compared with other fire retardants, with nanometer
Not only flame retarding efficiency is high for the fire retardant of level size, presses down cigarette, small toxicity, and can improve the compatibility with polymeric matrix.Will
It is introduced after polymeric system, and its peripheral particle can form stronger bonding action between organic phase, make polyhedral oligomeric sesquialter
There is good compatibility between Silicone particles and polymeric matrix, improve or eliminate reunion and two phase boundaries of inorganic particulate
The problem of face adhesion is weak, so as to improve the heat resistance of polymer.
The content of the invention
The technical problems to be solved by the invention are：A kind of nanometer for possessing both polymer and inorganic material advantage is provided
Structure fire retardant and preparation method thereof, to meet the use requirement under different condition to fire retardant.
To solve above-mentioned technical problem, the technical solution adopted by the present invention is as follows：
A kind of triguaiacyl phosphate polyhedral oligomeric sesquialter polysiloxanes fire retardant, with following structure：
A kind of method for preparing triguaiacyl phosphate polyhedral oligomeric sesquialter polysiloxanes fire retardant of the present invention, is with not complete
Seven phenyl silanetriol silsesquioxanes of full reduced conjunction carry out condensation reaction with diphenyl phosphate chloride in anhydrous tetrahydro furan and are made,
Its synthetic route is as follows：
Preferably, described condensation reaction is to carry out under nitrogen protection.
Preferably, described condensation reaction is stirring reaction 6~10 hours at 40~60 DEG C.
Preferably, terminate in described condensation reaction, reaction solution is filtered, filtrate is removed molten with distillation under vacuum
Agent, then neutrality is washed to distillation, dry.
As preferred scheme, count in mass ratio, the seven phenyl silanetriol silsesquioxanes: chlorine di(2-ethylhexyl)phosphate not being condensed completely
Phenyl ester: tetrahydrofuran=1：(0.89~2.18)：(10~50), wherein tetrahydrofuran need complete water removal.
Compared with prior art, the present invention has following conspicuousness progress：
The present invention is obtained by introducing three diphenyl phosphates in seven phenyl silanetriol silsesquioxanes not being condensed completely
Seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silesquioxane compounds have that relative molecular weight is big, phosphorus content is high, it is hot steady
Qualitative good, low cigarette, nontoxic, resistance to migration, the characteristic of resistance to volatilization, also with plasticising, it is heat-resisting, with the spy such as polymer matrix compatability is good
Point, can give full play to the advantage of polyhedral oligomeric sesquialter polysiloxanes and phosphate ester flame retardants, generate cooperative flame retardant effect, and
Preparation method is simple, performance is stable, with industrial applications value.
Brief description of the drawings
Fig. 1 is the synthetic route of fire retardant of the present invention；Wherein：Ith, seven phenyl silanetriol sesquialter silicon not being condensed completely
Oxygen alkane；IIth, diphenyl phosphate chloride；IIIth, fire retardant of the present invention：Seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes
Alkane；
Fig. 2 is seven phenyl silanetriol silsesquioxanes (I) not being condensed completely1H nuclear magnetic spectrums；
Fig. 3 is fire retardant of the present invention：Seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)1H cores
Magnetic chart is composed；
Fig. 4 is the infared spectrum for seven phenyl silanetriol silsesquioxanes (I) not being condensed completely；
Fig. 5 is fire retardant of the present invention：Seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III) it is infrared
Collection of illustrative plates；
Fig. 6 is fire retardant of the present invention：The heat mistake of seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)
Weight curve map.
Embodiment
With reference to embodiment, the present invention is described in further detail and completely.
Embodiment
1) preparation of seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)：
As shown in figure 1, the fire retardant that the present invention is provided：Seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)
Synthetic route be with the seven phenyl silanetriol silsesquioxanes (I) that are not condensed completely with diphenyl phosphate chloride (II) anhydrous four
Condensation reaction is carried out in hydrogen furans seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III) are made.
Specifically preparation process is：
Seven phenyl silanetriol silsesquioxanes (I), the chlorine phosphoric acid hexichol not being condensed completely are sequentially added in three-necked flask
Ester (II) and tetrahydrofuran anabolic reaction system, by suction filtration after reaction system stirring, heating, backflow, filtrate decompression is evaporated off molten
Agent, with distilled water flushing to pH ≈ 7, the light grey phenyl triphosphoric acid diphenyl ester of sticky matter fire retardant seven is produced after being then dried in vacuo
Polyhedral oligomeric silsesquioxane (III).
The phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxane (III) of three batch seven, preparation process are prepared in aforementioned manners
In material proportion and control parameter it is as shown in table 1：
Table 1
2) characterize data of seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)：
As shown in Fig. 2 being the seven phenyl silanetriol silsesquioxanes (I) that are not condensed completely1H nuclear magnetic spectrums；Fig. 3 institutes
Show, the phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxane (III) of fire retardant seven provided for the present invention1H nuclear magnetic spectrums.
From fig. 2 it can be seen that being about at 3.71, with obvious Si-OH peaks in ppm；It is phenyl ring at 7.15~7.85 to be in ppm
Environment residing for upper hydrogen；It is seen in figure 3 that due to not being condensed seven phenyl silanetriol silsesquioxanes (I) and chlorine phosphorus completely
Condensation reaction occurs for diphenyl phthalate (II), causes Si-OH peaks to disappear, therefore at it1On H nuclear magnetic spectrums only ppm be 6.95~
Occurs the collection of illustrative plates of hydrogen on phenyl ring at 7.85.
As shown in figure 4, the infrared light collection of illustrative plates for seven phenyl silanetriol silsesquioxanes (I) not being condensed completely；Shown in Fig. 5,
The infrared light collection of illustrative plates of the phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxane (III) of fire retardant seven provided for the present invention.By scheming
4 is visible, in about 1131cm-1Absworption peak of the place with polyhedral oligomeric sesquialter polysiloxanes Si-O-Si, about 3627cm-1Place has
Si-OH stretching vibration absworption peak, 898.7cm-1There is Si-OH flexural vibrations absworption peak；In fig. 5 it may be seen that about existing
1130cm-1There are polyhedral oligomeric sesquialter polysiloxanes Si-O-Si absworption peak, 1193cm in place-1There is the flexible of P=O to shake at left and right
Dynamic peak, 1027cm-1There are P-O stretching vibration peak, 954cm-1There is P-O-Si asymmetric stretching vibration peak.
3) physical characteristic of seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)：
A) average grain diameter：
The phenyl triphosphoric acid diphenyl ester polyhedral oligomeric sesquialter of fire retardant seven of three batches obtained with above-mentioned 1) preparation method
Siloxanes (III), after measured, with average grain diameter listed in such as table 2：
Table 2
From table 2：The fire retardant average grain diameter that the present invention is provided is 1.28~8.36nm, with nano-grade size knot
Structure, illustrates that seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III) and polymer have preferable compatibility.
B) thermal weight loss situation：
As shown in fig. 6, the phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxane of fire retardant seven provided for the present invention
(III) thermogravimetric curve figure, it is to use《Nano composite polymer/laminated silicate material theory and practice》(QiZongNeng,
Shang Wenyu writes, Chemical Industry Press, 2002) thermogravimetry detection is obtained as defined in.
Testing result shows, the phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxane of fire retardant seven that the present invention is provided
(III) decomposition temperature that thermal weight loss starts is 261.6 DEG C (weightlessness 5%)；Thermal decomposition process can be divided into for 2 stages, and the 1st stage existed
311.75 DEG C or so, now decomposition rate is most fast, but still has 71.53% quality remaining at 383.79 DEG C；2nd stage heat point
Solution appears in 500 DEG C or so, but still has at 700 DEG C 39.61% residual volume；Illustrate that the product has excellent heat resistance,
It can be directly applied to as fire retardant among other materials.
In summary, the fire retardant that the present invention is provided：Seven phenyl triphosphoric acid diphenyl ester polyhedral oligomeric silsesquioxanes (III)
With relative molecular weight is big, heat endurance is good and has preferable compatibility with polymer, has given full play to silicon-series five-retardant and phosphorus
The respective advantage of flame retardant, with good development prospect；In addition, the fire retardant that the present invention is provided：The phosphorus of seven phenyl three
The preparation method of diphenyl phthalate polyhedral oligomeric silsesquioxane is simple, performance is stable, with industrial application value.
Finally it is necessary described herein to be that the above embodiments are merely illustrative of the technical solutions of the present invention and unrestricted
Invention, although the present invention is described in detail with reference to preferred embodiment, it will be understood by those within the art that, can
Modified with the technical scheme to invention or equivalent substitution, without departing from the spirit and scope of technical solution of the present invention, its
It all should cover in scope of the presently claimed invention.
Claims (5)
1. a kind of preparation method of triguaiacyl phosphate polyhedral oligomeric sesquialter polysiloxanes fire retardant, described fire retardant has following knot
Structure：
It is characterized in that：The preparation method is with seven phenyl silicon three not being condensed completely
Alcohol silsesquioxane carries out condensation reaction with diphenyl phosphate chloride in anhydrous tetrahydro furan, and its synthetic route is as follows：
2. preparation method according to claim 1, it is characterised in that：Described condensation reaction is carried out under nitrogen protection.
3. preparation method according to claim 1, it is characterised in that：Described condensation reaction is stirred at 40~60 DEG C
Reaction 6~10 hours.
4. preparation method according to claim 1, it is characterised in that：Terminate in described condensation reaction, reaction solution is filtered
Cross, filtrate removes solvent with distillation under vacuum, then is washed to neutrality with distillation, dries.
5. the preparation method according to any one of Claims 1 to 4, it is characterised in that：Count, be not condensed completely in mass ratio
Seven phenyl silanetriol silsesquioxanes: diphenyl phosphate chloride: tetrahydrofuran=1：(0.89~2.18)：(10~50), wherein four
Hydrogen furans needs complete water removal.
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| CN109054023B (en) * | 2018-07-23 | 2021-02-12 | 德清顾舒家华高分子材料有限公司 | Preparation method of organic silicon-phosphorus synergistic flame retardant |
| CN109082106A (en) * | 2018-07-23 | 2018-12-25 | 德清顾舒家华高分子材料有限公司 | A kind of polyurethane foam containing organic silicon-phosphorus synergistic fire retardant |
| CN109096532A (en) * | 2018-08-20 | 2018-12-28 | 德清顾舒家华高分子材料有限公司 | A method of improving polyurethane foam flame retardant property |
| CN112280146A (en) * | 2020-10-27 | 2021-01-29 | 杭州富通通信技术股份有限公司 | Optical cable and preparation method thereof |
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