CN106268717A - A kind of preparation method of hexachlorocyclotriph,sphazene purification adsorbent - Google Patents
A kind of preparation method of hexachlorocyclotriph,sphazene purification adsorbent Download PDFInfo
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- CN106268717A CN106268717A CN201610691197.7A CN201610691197A CN106268717A CN 106268717 A CN106268717 A CN 106268717A CN 201610691197 A CN201610691197 A CN 201610691197A CN 106268717 A CN106268717 A CN 106268717A
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- hexachlorocyclotriph
- sphazene
- alcohol
- purification adsorbent
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 19
- 238000000746 purification Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 22
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 241000219289 Silene Species 0.000 claims abstract description 11
- 229910052918 calcium silicate Inorganic materials 0.000 claims abstract description 11
- 235000019439 ethyl acetate Nutrition 0.000 claims abstract description 10
- 150000001993 dienes Chemical class 0.000 claims abstract description 9
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 239000010936 titanium Substances 0.000 claims abstract description 7
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 claims abstract description 5
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- AYDQIZKZTQHYIY-UHFFFAOYSA-N OC(=O)C1(C)CC(C(O)=O)=CC=C1 Chemical compound OC(=O)C1(C)CC(C(O)=O)=CC=C1 AYDQIZKZTQHYIY-UHFFFAOYSA-N 0.000 claims description 6
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 108050008598 Phosphoesterases Proteins 0.000 claims description 2
- 239000004615 ingredient Substances 0.000 claims description 2
- ALSTYHKOOCGGFT-UHFFFAOYSA-N octadec-9-en-1-ol Chemical compound CCCCCCCCC=CCCCCCCCCO ALSTYHKOOCGGFT-UHFFFAOYSA-N 0.000 claims description 2
- -1 carbon tetraene Chemical class 0.000 abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract description 2
- MZPDTOMKQCMETI-YHYXMXQVSA-N (6z)-2,6-dimethylocta-2,6-diene Chemical compound C\C=C(\C)CCC=C(C)C MZPDTOMKQCMETI-YHYXMXQVSA-N 0.000 abstract 1
- 150000002576 ketones Chemical class 0.000 abstract 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 239000000047 product Substances 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 13
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Substances ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 4
- XCJXQCUJXDUNDN-UHFFFAOYSA-N chlordene Chemical compound C12C=CCC2C2(Cl)C(Cl)=C(Cl)C1(Cl)C2(Cl)Cl XCJXQCUJXDUNDN-UHFFFAOYSA-N 0.000 description 4
- QQVIHTHCMHWDBS-UHFFFAOYSA-N perisophthalic acid Natural products OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 4
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000006837 decompression Effects 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 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
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- MVPPADPHJFYWMZ-IDEBNGHGSA-N chlorobenzene Chemical group Cl[13C]1=[13CH][13CH]=[13CH][13CH]=[13CH]1 MVPPADPHJFYWMZ-IDEBNGHGSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000001514 detection method 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
- 239000012535 impurity 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
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 description 1
- 239000003444 phase transfer catalyst Substances 0.000 description 1
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000007870 radical polymerization initiator Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/264—Synthetic macromolecular compounds derived from different types of monomers, e.g. linear or branched copolymers, block copolymers, graft copolymers
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/18—Monomers containing fluorine
- C08F214/22—Vinylidene fluoride
- C08F214/225—Vinylidene fluoride with non-fluorinated comonomers
-
- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Polymers & Plastics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Medicinal Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention provides the preparation method of a kind of hexachlorocyclotriph,sphazene purification adsorbent: be distributed in water by a certain amount of vinylidene, it is proportionally added into (Z) 3, 7 dimethyl 2, 6 octadiene 1 alcohol acetic esters, 6, 10, 14, 18 tetramethyls 5, 9, 13, 170 nine carbon tetraene 2 ketone, Ammonium persulfate. and polyvinyl alcohol, 9 octadecylene 1 alcohol phosphate esters, 3 methyl 1, 5 di-p-tolyls 1, 4 pentaaza diene, four (trimethyl silene ether) titanium, heat up, react under preference temperature, product filters, dry, i.e. obtain hexachlorocyclotriph,sphazene purification adsorbent.
Description
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the system of a kind of hexachlorocyclotriph,sphazene purification adsorbent
Preparation Method.
Background technology
Hexachlorocyclotriph,sphazene, white powder crystal, density 1.98g/cm3, fusing point 112-115 DEG C, boiling point 256 DEG C.
Hexachlorocyclotriph,sphazene is high chlorine consuming products, and it is used as insecticide, fertilizer, antitumor drug, phase transfer catalyst, free radical
Polymerization initiator, light stabilizer, antioxidant, fire retardant etc..Can also be had the most widely by polyreaction complex functionality
Machine-inorganic macromolecule material, can be used for catalysis material, high-temperature resistant rubber, fire proofing, polyelectrolyte, photoconduction macromolecule
Material, nonlinear optical material, biological medical polymer material, high molecule liquid crystal, separation film, medicine, military project etc..Due to poly-phosphorus
The unique energy of nitrile material and added value are the highest, at present its synthesis and application are still that a study hotspot, and it is right to need
Hexachlorocyclotriph,sphazene and polyphosphazene material research and develop further.
CN103554186A discloses the preparation method of a kind of hexachlorocyclotriph,sphazene, and this preparation method is with zinc chloride, chlorination
Ferrum, magnesium chloride are composite catalyst, and with pyridine as acid binding agent, reaction temperature is 80～130 DEG C, and the response time is 6-10h；Reaction
Solvent is chlorobenzene.
CN104558044A discloses the synthetic method of a kind of hexachlorocyclotriph,sphazene, and it selects PCl5 and NH4Cl is at chlorobenzene
In solvent, react under catalyst existence condition, eventually pass filter, decompression distillation obtain hexachlorocyclotriph,sphazene crude product, will
Gained hexachlorocyclotriph,sphazene crude product is further dissolved in organic solvent, is recrystallized to give highly purified hexachlorocyclotriph,sphazene；Its
Comprise the steps of a. and be initially charged PCl in organic solvent5, stir with magnetic stirrer, add composite catalyst；Separately
Take NH4Cl and pyridine add in another container and stir, and are subsequently adding in reactor.B. highly purified chlordene is obtained after filtering
The chlorobenzene solution of ring three phosphonitrile, after decompression distills out chlorobenzene, obtains the thick product of phosphonitrile.
Existing hexachlorocyclotriph,sphazene purification is all by the physical method for separation such as recrystallization or distillation, inevitably
It is mixed into some impurity relying on physical method to remove.If carrying out primary sorption before physical purification method more, it is possible to
Obtain purity higher hexachlorocyclotriph,sphazene product.
Summary of the invention
It is an object of the invention to: providing the preparation method of a kind of hexachlorocyclotriph,sphazene purification adsorbent, it can be applied
In hexachlorocyclotriph,sphazene purification, its specific surface area is big, and adsorption rate is fast, and adsorbing contaminant amount is big, easy and simple to handle during application,
Adsorbed before hexachlorocyclotriph,sphazene recrystallization or distillation, the purity of hexachlorocyclotriph,sphazene product can be greatly promoted.
It is characterized in that preparation process includes:
A certain amount of vinylidene is distributed in water, adds (Z)-3,7-dimethyl-2,6-octadiene-1-in following ratio
Alcohol acetic ester, GGA, Ammonium persulfate. and polyvinyl alcohol, 9-ten
Eight alkene-1-alcohol phosphate esters, 3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, four-(trimethyl silene ether) titaniums, rise
Temperature, at 80-100 DEG C, reacts 14-20 hour, and product filters, and dries, i.e. obtains hexachlorocyclotriph,sphazene purification adsorbent.
Ingredients weight parts
Vinylidene 100
(Z)-3,7-dimethyl-2,6-octadiene-1-alcohol acetic ester 0.01-0.1
6,10,14,18-tetramethyl-5,9,13,17-19 carbon tetraene-2-ketone 0.01-0.1
Ammonium persulfate. 0.5-1.5
Polyvinyl alcohol 1.5-2.5
9-octadecene-1-ol phosphoesterase 30 .01-0.1
3-methyl isophthalic acid, 5-di-p-tolyl-1,4-pentaaza diene 0.1-0.5
Four-(trimethyl silene ether) titanium 0.5-1
Water 1000
Described (Z)-3,7-dimethyl-2,6-octadiene-1-alcohol acetic ester is commercially available prod, as think of sky, Chengdu moral biotechnology has
The product that limit company produces；GGA is commercially available prod, such as Hubei
The product that bright sunrise biochemistry pharmaceutcal corporation, Ltd produces, 9-octadecene-1-ol phosphate ester is commercially available prod, and sun chemical industry as big in Hangzhou has
The product that limit company produces；3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene is commercially available prod, as Tianjin Skien this
The product that biochemical technology company limited produces；Four-(trimethyl silene ether) titaniums are commercially available prod, such as Shanghai Chu Qing new material science and technology
The product that company limited produces.
The product of the present invention has the advantages that
Introduce (Z)-3,7-dimethyl-2,6-octadiene-1-alcohol acetic ester, 6,10,14,18-tetramethyl-5,9,13,17-ten
Nine carbon tetraene-2-ketone, 9-octadecene-1-ol phosphate ester, 3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, four-(three
Methyl silene ether) titanium is as polymerization monomer, and adsorbent has higher heat stability and chemical stability, specific surface area height, inhales
Attached speed is fast, and the amount of adsorbing contaminant is big.Apply this adsorbent after purifying, to carry out the physical method for separation purification such as crystallization again to produce
Product, the hexachlorocyclotriph,sphazene product purity obtained is higher.
Detailed description of the invention
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
In 2000L reactor, add 100Kg vinylidene chloride, 1000Kg water, 0.05Kg (Z)-3,7-dimethyl-2,6-pungent two
Alkene-1-alcohol acetic ester, 0.05Kg6,10,14,18-tetramethyl-5,9,13,17-ten nine carbon tetraene-2-ketone, 1Kg Ammonium persulfate.,
2Kg polyvinyl alcohol, 0.05Kg9-octadecene-1-ol phosphate ester, 0.3Kg3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza two
Alkene, 0.8Kg tetra--(trimethyl silene ether) titanium, it is warming up to 90 DEG C, reacts 17h, product filters, and dries, i.e. obtains chlordene ring three phosphorus
Nitrile purification adsorbent.
Embodiment 2
In 2000L reactor, add 100Kg vinylidene chloride, 1000Kg water, 0.01Kg (Z)-3,7-dimethyl-2,6-pungent two
Alkene-1-alcohol acetic ester, 0.01Kg6,10,14,18-tetramethyl-5,9,13,17-ten nine carbon tetraene-2-ketone, 0.5Kg persulfuric acid
Ammonium, 1.5Kg polyvinyl alcohol, 0.01Kg9-octadecene-1-ol phosphate ester, 0.1Kg3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-five
Aza-diene, 0.5Kg tetra--(trimethyl silene ether) titanium, it is warming up to 80 DEG C, reacts 14h, product filters, and dries, i.e. obtains chlordene
Ring three phosphonitrile purification adsorbent.
Embodiment 3
In 2000L reactor, add 100Kg vinylidene chloride, 1000Kg water, 0.1Kg (Z)-3,7-dimethyl-2,6-pungent two
Alkene-1-alcohol acetic ester, 0.1Kg6,10,14,18-tetramethyl-5,9,13,17-ten nine carbon tetraene-2-ketone, 1.5Kg Ammonium persulfate.,
2.5Kg polyvinyl alcohol, 0.1Kg9-octadecene-1-ol phosphate ester, 0.5Kg3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza
Diene, 0.5Kg tetra--(trimethyl silene ether) titanium, it is warming up to 100 DEG C, reacts 20h, product filters, and dries, i.e. obtains chlordene ring
Three phosphonitrile purification adsorbents.
Comparative example 1
Being added without (Z)-3,7-dimethyl-2,6-octadiene-1-alcohol acetic ester, other conditions are with embodiment 1.
Comparative example 2
Being added without GGA, other conditions are with embodiment 1.
Comparative example 3
Being added without 9-octadecene-1-ol phosphate ester, other conditions are with embodiment 1.
Comparative example 4
Being added without 3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, other conditions are with embodiment 1.
Comparative example 5
Being added without four-(trimethyl silene ether) titaniums, other conditions are with embodiment 1.
Comparative example 6
It is added without the adsorbent product that the present invention is produced, adsorbs with activated carbon.
Embodiment 4
The hexachlorocyclotriph,sphazene crude product that purity is 99% is passed through the adsorbent made equipped with 500g embodiment 1-3 and comparative example 1-6
In the 1000mL exchange column of product, temperature 80 DEG C, flow velocity 0.5BV/h, under the conditions of absorption purify, use gas chromatographic detection effluent
Weight/mass percentage composition, be shown in Table 1.
Table 1: the hexachlorocyclotriph,sphazene purity after the hexachlorocyclotriph,sphazene adsorbent purification that different process is produced.
| Numbering | Hexachlorocyclotriph,sphazene purity (%) |
| Embodiment 1 | 99.31 |
| Embodiment 2 | 99.19 |
| Embodiment 3 | 99.49 |
| Comparative example 1 | 99.11 |
| Comparative example 2 | 99.09 |
| Comparative example 3 | 99.07 |
| Comparative example 4 | 99.12 |
| Comparative example 5 | 99.10 |
| Comparative example 6 | 99.07 |
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with this
Based on bright, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (2)
1. a hexachlorocyclotriph,sphazene purification adsorbent, it is characterised in that include following material component:
Ingredients weight parts
Vinylidene 100
(Z)-3,7-dimethyl-2,6-octadiene-1-alcohol acetic ester 0.01-0.1
6,10,14,18-tetramethyl-5,9,13,17-19 carbon tetraene-2-ketone 0.01-0.1
Ammonium persulfate. 0.5-1.5
Polyvinyl alcohol 1.5-2.5
9-octadecene-1-ol phosphoesterase 30 .01-0.1
3-methyl isophthalic acid, 5-di-p-tolyl-1,4-pentaaza diene 0.1-0.5
Four-(trimethyl silene ether) titanium 0.5-1
Water 1000.
2. the preparation method of a hexachlorocyclotriph,sphazene purification adsorbent, it is characterised in that comprise the following steps:
A certain amount of vinylidene is distributed in water, is proportionally added into (Z)-3,7-dimethyl-2,6-octadiene-1-alcohol acetic acid
Ester, GGA, Ammonium persulfate. and polyvinyl alcohol, 9-octadecylene-
1-alcohol phosphate ester, 3-methyl isophthalic acid, 5-di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, four-(trimethyl silene ether) titaniums, heat up,
80-100 DEG C, reacting 14-20 hour, product filters, and dries, i.e. obtains hexachlorocyclotriph,sphazene purification adsorbent.
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| CN201710410684.6A CN107011385A (en) | 2016-08-21 | 2017-06-04 | A kind of hexachlorocyclotriph,sphazene purifies the preparation method of auxiliary agent |
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| CN110903646A (en) * | 2019-12-11 | 2020-03-24 | 南通双晨新材料科技有限公司 | Preparation method of nylon cable tie material with high and low temperature resistance |
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| US4175113A (en) * | 1978-04-20 | 1979-11-20 | The Firestone Tire & Rubber Company | Purification of crude chlorophosphazene compounds by treatment with water |
| US20110124819A1 (en) * | 2008-04-25 | 2011-05-26 | Basf Se | Modified halogenated polymer surfaces |
| CN104558044A (en) * | 2015-02-13 | 2015-04-29 | 湖北诺邦科技股份有限公司 | Synthesis method of hexachlorocyclotriphosphazene |
| CN105582901B (en) * | 2015-12-21 | 2018-03-02 | 王金明 | A kind of preparation of the adsorbent of long carbochain biatomic acid zymotic fluid |
| CN105597711B (en) * | 2016-03-09 | 2018-11-23 | 徐州鸿丰高分子材料有限公司 | A kind of preparation method of the adsorbent material of binary acid treating |
| CN105727686B (en) * | 2016-03-25 | 2017-12-08 | 张玲 | A kind of method for adsorbing purification sulfur hexafluoride |
| CN105668639B (en) * | 2016-04-05 | 2017-06-13 | 浙江博瑞电子科技有限公司 | A kind of method for adsorbing purification tungsten hexafluoride |
| CN105753819B (en) * | 2016-04-26 | 2018-06-08 | 张玲 | A kind of method of 5 hydroxymethyl furfural purifying |
| CN105801474B (en) * | 2016-05-26 | 2018-01-16 | 张玲 | A kind of method of refined 3,6 lontrel |
| CN105777970A (en) * | 2016-05-27 | 2016-07-20 | 张玲 | Preparation method of adsorbent for refining trimesic acid |
| CN105859938A (en) * | 2016-06-13 | 2016-08-17 | 王金明 | Preparation of cobalt adsorbent |
| CN105833854A (en) * | 2016-06-13 | 2016-08-10 | 王金明 | Preparation method of purified vanadium adsorption material |
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| CN110903646A (en) * | 2019-12-11 | 2020-03-24 | 南通双晨新材料科技有限公司 | Preparation method of nylon cable tie material with high and low temperature resistance |
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