CN107930589A - A kind of preparation method of hexachlorocyclotriph,sphazene upgrading material - Google Patents
A kind of preparation method of hexachlorocyclotriph,sphazene upgrading material Download PDFInfo
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- CN107930589A CN107930589A CN201711189534.3A CN201711189534A CN107930589A CN 107930589 A CN107930589 A CN 107930589A CN 201711189534 A CN201711189534 A CN 201711189534A CN 107930589 A CN107930589 A CN 107930589A
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- hexachlorocyclotriph
- sphazene
- glass beads
- porous glass
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- 239000000463 material Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000011324 bead Substances 0.000 claims abstract description 29
- 239000005373 porous glass Substances 0.000 claims abstract description 29
- 108010010803 Gelatin Proteins 0.000 claims abstract description 10
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 10
- 229920000159 gelatin Polymers 0.000 claims abstract description 10
- 239000008273 gelatin Substances 0.000 claims abstract description 10
- 235000019322 gelatine Nutrition 0.000 claims abstract description 10
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 10
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 claims abstract description 10
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 9
- NWQIWFOQNHTTIA-UHFFFAOYSA-N diethoxy-bis(prop-2-enyl)silane Chemical compound CCO[Si](CC=C)(CC=C)OCC NWQIWFOQNHTTIA-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940117958 vinyl acetate Drugs 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- MWQKURVBJZAOSC-UHFFFAOYSA-N 1-propan-2-ylcyclopenta-1,3-diene Chemical class CC(C)C1=CC=CC1 MWQKURVBJZAOSC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- OILUAKBAMVLXGF-UHFFFAOYSA-N 3,5,5-trimethyl-hexanoic acid Chemical class OC(=O)CC(C)CC(C)(C)C OILUAKBAMVLXGF-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000010792 warming Methods 0.000 claims description 5
- JIXZZWAATLXBBG-UHFFFAOYSA-N 1-chloro-1-ethenylsiletane Chemical compound C=C[Si]1(Cl)CCC1 JIXZZWAATLXBBG-UHFFFAOYSA-N 0.000 claims description 3
- PMJHHCWVYXUKFD-SNAWJCMRSA-N (E)-1,3-pentadiene Chemical compound C\C=C\C=C PMJHHCWVYXUKFD-SNAWJCMRSA-N 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- -1 chlorovinyl Chemical group 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 239000012043 crude product Substances 0.000 description 4
- OILUAKBAMVLXGF-UHFFFAOYSA-M 3,5,5-trimethylhexanoate Chemical compound [O-]C(=O)CC(C)CC(C)(C)C OILUAKBAMVLXGF-UHFFFAOYSA-M 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 235000019270 ammonium chloride Nutrition 0.000 description 3
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 3
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 239000002841 Lewis acid Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 description 2
- 150000007517 lewis acids Chemical class 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- YDUIJCOOKSZFBO-UHFFFAOYSA-N 1-(1-chloroethenyl)siletane Chemical compound ClC(=C)[SiH]1CCC1 YDUIJCOOKSZFBO-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 1
- 241000255964 Pieridae Species 0.000 description 1
- GJMMXPXHXFHBPK-UHFFFAOYSA-N [P].[Cl] Chemical compound [P].[Cl] GJMMXPXHXFHBPK-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002246 antineoplastic agent Substances 0.000 description 1
- 229940041181 antineoplastic drug Drugs 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N n-pentane Natural products CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000003444 phase transfer catalyst Substances 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 239000007870 radical polymerization initiator Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- QZYLHXTXFGOILC-UHFFFAOYSA-N siletane Chemical compound C1C[SiH2]C1 QZYLHXTXFGOILC-UHFFFAOYSA-N 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6581—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and nitrogen atoms with or without oxygen or sulfur atoms, as ring hetero atoms
- C07F9/65812—Cyclic phosphazenes [P=N-]n, n>=3
- C07F9/65815—Cyclic phosphazenes [P=N-]n, n>=3 n = 3
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a kind of preparation method of hexachlorocyclotriph,sphazene upgrading material.By weight, porous glass beads, vinylacetate are added in a kettle, diallyl diethoxy silane, 1 chlorovinyl silacyclobutane, gelatin, 1 pi-allyl, 3 vinyl imidazole trifluoromethanesulfonimide salt, three (isopropylcyclopentadienes) change neodymium, peroxidating 3,5,5 trimethylhexanoates, water, heating, reaction, isolates the porous glass beads through surface aggregate after reaction, washing, it is dry, that is, obtain hexachlorocyclotriph,sphazene upgrading material.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of preparation side of hexachlorocyclotriph,sphazene upgrading material
Method.
Background technology
Hexachlorocyclotriph,sphazene easily distils, its steam has stimulation to eyes and respiratory tract.It is dissolvable in water most of organic
In solvent, such as normal heptane, benzene, petroleum ether.Due to the activity of phosphorus chlorine key, chlorine can be made to be easy to be substituted, just because of
This reason, can be made a series of phosphazene compound.Additionally, due to the stability of hexatomic ring, make it have acidproof, alkaline-resisting
And high-temperature stability.It is used as insecticide, fertilizer, antitumor drug, phase transfer catalyst, radical polymerization initiator, light
Stabilizer, antioxidant, fire retardant etc..The more extensive organic and inorganic macromolecule of polymerisation complex functionality can also be passed through
Material, available for catalysis material, high-temperature resistant rubber, fire proofing, polyelectrolyte, light guide high molecular material, nonlinear optical
Learn material, biological medical polymer material, high molecule liquid crystal, seperation film, medicine, military project etc..
CN104558044A discloses a kind of synthetic method of hexachlorocyclotriph,sphazene, it selects PCl5 and NH4Cl in chlorobenzene
In solvent, react under catalyst existence condition, last filtered, vacuum distillation obtains hexachlorocyclotriph,sphazene crude product, will
Gained hexachlorocyclotriph,sphazene crude product is further dissolved in organic solvent, is recrystallized to give the hexachlorocyclotriph,sphazene of high-purity；Its
Comprise the steps of：A. PCl5 is first added in organic solvent, is stirred evenly with magnetic stirrer, adds composite catalyst；Separately
Take NH4Cl and pyridine to add in another container and stir evenly, then add in reaction kettle.B. the chlordene of high-purity is obtained after filtering
The chlorobenzene solution of three phosphonitrile of ring, after being evaporated under reduced pressure out chlorobenzene, obtains phosphonitrile crude product.
CN103570763A is disclosed one kind and is synthesized with Lewis acid for catalyst and using sublimed method purifying chlordene ring
The new process of tripolyphosphazene.The feature of this method is catalyst selecting Lewis acid, is existed using ammonium chloride and phosphorus pentachloride as raw material
Chlorobenzene is to synthesize hexa chloro cyclotripolyphosphazene in solvent, and is removed linearly with n-hexane dissolution hexa chloro cyclotripolyphosphazene after removing chlorobenzene
Polymer.
Existing hexachlorocyclotriph,sphazene must prepare or purify public good, be purified mostly using the methods of recrystallization, distillation,
Purifying technique elapsed time is grown, and technique is cumbersome, and consumed energy is big.Therefore, a kind of new hexachlorocyclotriph,sphazene upgrading material is researched and developed
It is necessary.
The content of the invention
The purpose of the present invention is：There is provided a kind of preparation method of hexachlorocyclotriph,sphazene upgrading material, it is characterised in that prepare
Step includes：
By weight, porous glass beads, vinylacetate, diallyl diethoxy silane, 1- are added in a kettle
Chloro- vinyl-silacyclobutane, gelatin, 1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt, three (isopropyl basic rings
Pentadiene) change neodymium, peroxidating 3,5,5- trimethylhexanoates, water, is warming up to 75-85 DEG C, reacts 8-15h, and reaction terminates
The porous glass beads through surface aggregate are isolated afterwards, are washed, it is dry, that is, obtain hexachlorocyclotriph,sphazene upgrading material.
The vinylacetate, its quality dosage are the 5-15% of porous glass beads.
The diallyl diethoxy silane, its quality dosage are the 1-2% of porous glass beads.
Chloro- vinyl-the silacyclobutanes of the 1-, its quality dosage are the 0.5-1% of porous glass beads.
The gelatin, its quality dosage are the 0.1-0.5% of porous glass beads.
1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide the salt, its quality dosage are micro- for cellular glass
The 0.1-0.3% of pearl.
Three (isopropylcyclopentadienes) change neodymium, its quality dosage is the 0.01-0.1% of porous glass beads.
3,5, the 5- trimethylhexanoate of peroxidating, its quality dosage are the 0.5- of porous glass beads
1.5%。
The water, its quality dosage are the 400-700% of porous glass beads.
The porous glass beads, vinylacetate, diallyl diethoxy silane, the chloro- vinyl of 1--sila ring
Butane, gelatin, 1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt, three (isopropylcyclopentadienes) change neodymium, peroxide
Change 3,5,5- trimethylhexanoates, be commercial product.
The product of the present invention has the advantages that：
The hexachlorocyclotriph,sphazene upgrading material that the present invention is produced, it is not easily to fall off in the close load in porous glass beads surface, can
With the performance efficacy of adsorption of long-acting stabilization；It is fast with adsorption rate, the advantages of adsorption capacity is big, and service life is long, greatly reduce
The time consumption and resource cost of purification link.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
In a kettle, porous glass beads 100Kg, vinylacetate 10Kg, diallyl diethoxy silane are added
1.5Kg, 1- chloro- vinyl-silacyclobutane 0.75Kg, gelatin 0.3Kg, 1- pi-allyl -3- vinyl imidazole fluoroform sulphurs
Imide salts 0.2Kg, three (isopropylcyclopentadienes) change neodymium 0.05Kg, peroxidating 3,5,5- trimethylhexanoate 1Kg, water
550Kg, is warming up to 80 DEG C, reacts 11.5h, isolates the porous glass beads through surface aggregate after reaction, washes, and does
It is dry, that is, obtain hexachlorocyclotriph,sphazene upgrading material.
Embodiment 2
In a kettle, porous glass beads 100Kg, vinylacetate 5Kg, diallyl diethoxy silane 1Kg, 1- are added
Chloro- vinyl-silacyclobutane 0.5Kg, gelatin 0.1Kg, 1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt
0.1Kg, three (isopropylcyclopentadienes) change neodymium 0.01Kg, peroxidating 3,5,5- trimethylhexanoate 0.5Kg, water 400Kg,
75 DEG C are warming up to, 8h is reacted, isolates the porous glass beads through surface aggregate after reaction, is washed, it is dry, that is, obtain six
Three phosphonitrile upgrading material of chlorine ring.
Embodiment 3
In a kettle, porous glass beads 100Kg, vinylacetate 15Kg, diallyl diethoxy silane 2Kg are added,
The chloro- vinyl of 1--silacyclobutane 1Kg, gelatin 0.5Kg, 1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt
0.3Kg, three (isopropylcyclopentadienes) change neodymium 0.1Kg, peroxidating 3,5,5- trimethylhexanoate 1.5Kg, water 700Kg,
85 DEG C are warming up to, 15h is reacted, isolates the porous glass beads through surface aggregate after reaction, is washed, it is dry, that is, obtain
Hexachlorocyclotriph,sphazene upgrading material.
Comparative example 1
Chloro- vinyl-the silacyclobutanes of 1- are added without, other conditions are the same as embodiment 1.
Comparative example 2
Gelatin is added without, other conditions are the same as embodiment 1.
Comparative example 3
1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt is added without, other conditions are the same as embodiment 1.
Comparative example 4
It is added without three (isopropylcyclopentadienes) and changes neodymium, other conditions is the same as embodiment 1.
Embodiment 4
The hexachlorocyclotriph,sphazene crude product that purity is 99% is passed through to the adsorbent made equipped with 500g embodiments 1-3 and comparative example 1-6
In the 1000mL exchange columns of product, 80 DEG C, flow velocity 0.5BV/h of temperature, under the conditions of adsorb purification, with gas chromatographic detection efflux
Mass percentage, be shown in Table 1.
Table 1：Hexachlorocyclotriph,sphazene purity after the hexachlorocyclotriph,sphazene upgrading material absorption purification that different process is produced.
Claims (9)
1. a kind of preparation method of hexachlorocyclotriph,sphazene upgrading material, it is characterised in that include the following steps：
By weight, porous glass beads, vinylacetate, diallyl diethoxy silane, 1- are added in a kettle
Chloro- vinyl-silacyclobutane, gelatin, 1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt, three (isopropyl basic rings
Pentadiene) change neodymium, peroxidating 3,5,5- trimethylhexanoates, water, is warming up to 75-85 DEG C, reacts 8-15h, and reaction terminates
The porous glass beads through surface aggregate are isolated afterwards, are washed, it is dry, that is, obtain hexachlorocyclotriph,sphazene upgrading material.
A kind of 2. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Vinylacetate, its quality dosage are the 5-15% of porous glass beads.
A kind of 3. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Diallyl diethoxy silane, its quality dosage are the 1-2% of porous glass beads.
A kind of 4. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Chloro- vinyl-the silacyclobutanes of 1-, its quality dosage are the 0.5-1% of porous glass beads.
A kind of 5. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Gelatin, its quality dosage are the 0.1-0.5% of porous glass beads.
A kind of 6. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
1- pi-allyl -3- vinyl imidazole trifluoromethanesulfonimide salt, its quality dosage are the 0.1-0.3% of porous glass beads.
A kind of 7. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Three (isopropylcyclopentadienes) change neodymium, its quality dosage is the 0.01-0.1% of porous glass beads.
A kind of 8. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Peroxidating 3,5,5- trimethylhexanoates, its quality dosage are the 0.5-1.5% of porous glass beads.
A kind of 9. preparation method of hexachlorocyclotriph,sphazene upgrading material according to claim 1, it is characterised in that：Described
Water, its quality dosage are the 400-700% of porous glass beads.
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| CN201711189534.3A CN107930589A (en) | 2017-11-24 | 2017-11-24 | A kind of preparation method of hexachlorocyclotriph,sphazene upgrading material |
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Application publication date: 20180420 |