CN107011385A - A kind of hexachlorocyclotriph,sphazene purifies the preparation method of auxiliary agent - Google Patents
A kind of hexachlorocyclotriph,sphazene purifies the preparation method of auxiliary agent Download PDFInfo
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- CN107011385A CN107011385A CN201710410684.6A CN201710410684A CN107011385A CN 107011385 A CN107011385 A CN 107011385A CN 201710410684 A CN201710410684 A CN 201710410684A CN 107011385 A CN107011385 A CN 107011385A
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- Prior art keywords
- hexachlorocyclotriph
- sphazene
- alcohol
- auxiliary agent
- purifies
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- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 13
- 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
- -1 carbon tetraene Chemical class 0.000 claims abstract description 13
- 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 11
- 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 10
- 150000001993 dienes Chemical class 0.000 claims abstract description 9
- 238000000746 purification Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 7
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 5
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 7
- 239000010936 titanium Substances 0.000 claims description 7
- 229910052719 titanium Inorganic materials 0.000 claims description 7
- MZPDTOMKQCMETI-YHYXMXQVSA-N (6z)-2,6-dimethylocta-2,6-diene Chemical class C\C=C(\C)CCC=C(C)C MZPDTOMKQCMETI-YHYXMXQVSA-N 0.000 claims description 6
- AYDQIZKZTQHYIY-UHFFFAOYSA-N OC(=O)C1(C)CC(C(O)=O)=CC=C1 Chemical class OC(=O)C1(C)CC(C(O)=O)=CC=C1 AYDQIZKZTQHYIY-UHFFFAOYSA-N 0.000 claims description 6
- 150000001336 alkenes Chemical class 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 235000021317 phosphate Nutrition 0.000 claims description 6
- 108050008598 Phosphoesterases Proteins 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 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
- 239000004698 Polyethylene Substances 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 abstract description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 abstract description 2
- 239000010452 phosphate Substances 0.000 abstract description 2
- GDDAJHJRAKOILH-QFXXITGJSA-N (2e,5e)-octa-2,5-diene Chemical compound CC\C=C\C\C=C\C GDDAJHJRAKOILH-QFXXITGJSA-N 0.000 abstract 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 150000002576 ketones Chemical class 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 abstract 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 abstract 1
- 239000000047 product Substances 0.000 description 17
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Substances ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- ZSTLPJLUQNQBDQ-UHFFFAOYSA-N azanylidyne(dihydroxy)-$l^{5}-phosphane Chemical compound OP(O)#N ZSTLPJLUQNQBDQ-UHFFFAOYSA-N 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 4
- 239000003463 adsorbent Substances 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
- 239000012043 crude product Substances 0.000 description 4
- LGXVIGDEPROXKC-UHFFFAOYSA-N 1,1-dichloroethene Chemical class ClC(Cl)=C LGXVIGDEPROXKC-UHFFFAOYSA-N 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 3
- 238000000053 physical 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
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000019270 ammonium chloride Nutrition 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- MEESPVWIOBCLJW-UHFFFAOYSA-N octadec-9-enyl dihydrogen phosphate Chemical class CCCCCCCCC=CCCCCCCCCOP(O)(O)=O MEESPVWIOBCLJW-UHFFFAOYSA-N 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- UHZYTMXLRWXGPK-UHFFFAOYSA-N phosphorus pentachloride Chemical compound ClP(Cl)(Cl)(Cl)Cl UHZYTMXLRWXGPK-UHFFFAOYSA-N 0.000 description 2
- 229920002627 poly(phosphazenes) Polymers 0.000 description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005292 vacuum distillation Methods 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
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000118 anti-neoplastic effect Effects 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
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic 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
- 238000001514 detection method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003337 fertilizer Substances 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
- 239000003999 initiator Substances 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 239000007788 liquid 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
- 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
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring 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
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- 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
-
- 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
-
- 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)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention provides the preparation method that a kind of hexachlorocyclotriph,sphazene purifies auxiliary agent, it is characterised in that comprises the following steps：A certain amount of vinylidene is distributed in water, the ratio according to claim 1 adds (Z) 3,7 dimethyl 2, the alcohol acetic ester of 6 octadiene 1,6,10,14,18 tetramethyls 5,9,13, the ketone of 170 nine carbon tetraene 2, ammonium persulfate and polyvinyl alcohol, the alcohol phosphate of 9 octadecylene 1, the di-p-tolyl 1 of 3 methyl 1,5,4 pentaaza diene, four (trimethyl silene ether) titaniums, heating, at 80 100 DEG C, react 14 20 hours, product is filtered, drying, that is, obtains hexachlorocyclotriph,sphazene purification auxiliary agent.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of hexachlorocyclotriph,sphazene purifies the preparation side of auxiliary agent
Method.Background technology
Hexachlorocyclotriph,sphazene, white powder crystal, density 1.98g/cm3,112-115 DEG C of fusing point, 256 DEG C of boiling point.Six
The phosphonitrile of chlorine ring three is high chlorine consuming products, and it is used as insecticide, fertilizer, antineoplastic, phase transfer catalyst, radical polymerization
Close initiator, light stabilizer, antioxidant, fire retardant etc..Can also by polymerisation complex functionality more it is extensive it is organic-
Inorganic macromolecule material, available for catalysis material, high-temperature resistant rubber, fire proofing, polyelectrolyte, light guide macromolecule material
Material, nonlinear optical material, biological medical polymer material, high molecule liquid crystal, seperation film, medicine, military project etc..Due to polyphosphazene
Material it is unique can and added value is all very high, it is synthesized at present and using being still a study hotspot, it is necessary to six
The phosphonitrile of chlorine ring three and polyphosphazene material are further researched and developed.
CN103554186A discloses a kind of preparation method of hexachlorocyclotriph,sphazene, and the preparation method is with zinc chloride, chlorination
Iron, magnesium chloride are composite catalyst, using pyridine as acid binding agent, and reaction temperature is 80~130 DEG C, and the reaction time is 6-10h；Reaction
Solvent is chlorobenzene.
CN104558044A discloses a kind of synthetic method of hexachlorocyclotriph,sphazene, and it is from PCl5 and NH4Cl in chlorobenzene
In solvent, reacted under catalyst existence condition, eventually pass filter, vacuum distillation and obtain 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 with magnetic stirrer, adds composite catalyst；Separately
Take NH4Cl and pyridine to add to stir in another container, then add in reactor.B. the chlordene of high-purity is obtained after filtering
The chlorobenzene solution of the phosphonitrile of ring three, vacuum distillation goes out after chlorobenzene, obtains phosphonitrile crude product.
The purifying of existing hexachlorocyclotriph,sphazene is all by recrystallization or the physical method for separation such as distil, inevitably
It is mixed into some impurity for relying on physical method not remove.If many before physical purification method once adsorbed, it is possible to
Obtain the higher hexachlorocyclotriph,sphazene product of purity.
The content of the invention
The purpose of the present invention is：The preparation method that a kind of hexachlorocyclotriph,sphazene purifies auxiliary agent is provided, it can apply to six
In the phosphonitrile purification of chlorine ring three, its specific surface area is big, and adsorption rate is fast, and adsorbing contaminant amount is big, using when it is easy to operate, use
Adsorbed before hexachlorocyclotriph,sphazene is recrystallized or is distilled, the purity of hexachlorocyclotriph,sphazene product can be greatly promoted.Its
It is characterised by that preparation process includes：
A certain amount of vinylidene is distributed in water, (Z) -3,7- dimethyl -2,6- octadienes -1- is added in following ratios
Alcohol acetic ester, GGA, ammonium persulfate and polyvinyl alcohol, 9- ten
Eight alkene -1- alcohol phosphates, 3- methyl isophthalic acids, 5- di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, four-(trimethyl silene ether) titaniums rise
Temperature, at 80-100 DEG C, reacts 14-20 hours, product filtering, drying, that is, obtains hexachlorocyclotriph,sphazene purification auxiliary agent.
Ingredients weight parts
Vinylidene 100
(Z) -3,7- dimethyl -2,6- octadienes -1- alcohol acetic esters 0.01-0.1
Carbon tetraene -2- ketone the 0.01-0.1 of 6,10,14,18- tetramethyls -5,9,13,17- 19
Ammonium persulfate 0.5-1.5
Polyvinyl alcohol 1.5-2.5
9- octadecene-1-ol phosphoesterase 30s .01-0.1
3- methyl isophthalic acids, 5- di-p-tolyl -1,4- pentaaza diene 0.1-0.5
Four-(trimethyl silene ether) titanium 0.5-1
Water 1000
(Z) -3,7- dimethyl -2,6- octadiene -1- alcohol acetic esters are commercially available prod, and such as day moral biotechnology is thought in Chengdu has
The product of limit company production；GGA is commercially available prod, such as Hubei
The product of the biochemical pharmaceutcal corporation, Ltd's production of bright sunrise, 9- octadecene-1-ols phosphate is commercially available prod, and the big positive chemical industry in such as Hangzhou has
The product of limit company production；3- methyl isophthalic acids, 5- di-p-tolyl-Isosorbide-5-Nitraes-pentaaza diene be commercially available prod, such as Tianjin Skien this
The product of biochemical technology Co., Ltd production；Four-(trimethyl silene ether) titaniums are commercially available prod, such as Shanghai Chu Qing new materials science and technology
The product of Co., Ltd's production.
The product of the present invention has the advantages that：
Introduce (Z) -3,7- dimethyl -2,6- octadiene -1- alcohol acetic esters, 6,10,14,18- tetramethyls -5,9,13,17- ten
Nine carbon tetraene -2- ketone, 9- octadecene-1-ol phosphates, 3- methyl isophthalic acids, 5- di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, four-(three
Methyl silene ether) titanium is as polymerized monomer, and adsorbent has stronger heat endurance and chemical stability, and specific surface area is high, inhales
Attached speed is fast, and the amount of adsorbing contaminant is big.Carry out the physical method for separation purifying production such as crystallizing again after purifying using the absorption of this adsorbent
Product, obtained hexachlorocyclotriph,sphazene product purity is higher.
Embodiment
Following instance is only to further illustrate the present invention, is not limitation the scope of protection of the invention.
Embodiment 1
In 2000L reactors, 100Kg vinylidene chlorides, 1000Kg water, 0.05Kg (Z) -3,7- dimethyl -2,6- pungent two are added
Alkene -1- alcohol acetic esters, 0.05Kg6,10,14,18- tetramethyls -5,9,13,17- ten nine carbon tetraene -2- ketone, 1Kg ammonium persulfates,
2Kg polyvinyl alcohol, 0.05Kg9- octadecene-1-ol phosphates, 0.3Kg3- methyl isophthalic acids, 5- di-p-tolyls-Isosorbide-5-Nitrae-pentaaza two
Alkene, 0.8Kg tetra--(trimethyl silene ether) titanium is warming up to 90 DEG C, reacts 17h, and product filtering, drying obtains the phosphorus of chlordene ring three
Nitrile purifies auxiliary agent.
Embodiment 2
In 2000L reactors, 100Kg vinylidene chlorides, 1000Kg water, 0.01Kg (Z) -3,7- dimethyl -2,6- pungent two are added
Alkene -1- alcohol acetic esters, 0.01Kg6,10,14,18- tetramethyls -5,9,13,17- ten nine carbon tetraene -2- ketone, 0.5Kg persulfuric acid
Ammonium, 1.5Kg polyvinyl alcohol, 0.01Kg9- octadecene-1-ol phosphates, 0.1Kg3- methyl isophthalic acids, 5- di-p-tolyls-Isosorbide-5-Nitrae-five
Aza-diene, 0.5Kg tetra--(trimethyl silene ether) titanium is warming up to 80 DEG C, reacts 14h, and product filtering, drying obtains chlordene
The phosphonitrile of ring three purifies auxiliary agent.
Embodiment 3
In 2000L reactors, 100Kg vinylidene chlorides, 1000Kg water, 0.1Kg (Z) -3,7- dimethyl -2,6- pungent two are added
Alkene -1- alcohol acetic esters, 0.1Kg6,10,14,18- tetramethyls -5,9,13,17- ten nine carbon tetraene -2- ketone, 1.5Kg ammonium persulfates,
2.5Kg polyvinyl alcohol, 0.1Kg9- octadecene-1-ol phosphates, 0.5Kg3- methyl isophthalic acids, 5- di-p-tolyls-Isosorbide-5-Nitrae-pentaaza
Diene, 0.5Kg tetra--(trimethyl silene ether) titanium is warming up to 100 DEG C, reacts 20h, and product filtering, drying obtains chlordene ring
Three phosphonitriles purify auxiliary agent.
Comparative example 1
It is added without (Z) -3,7- dimethyl -2,6- octadiene -1- alcohol acetic esters, other conditions be the same as Example 1.
Comparative example 2
It is added without GGA, other conditions be the same as Example 1.
Comparative example 3
It is added without 9- octadecene-1-ol phosphates, other conditions be the same as Example 1.
Comparative example 4
It is added without 3- methyl isophthalic acids, 5- di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, other conditions be the same as Example 1.
Comparative example 5
It is added without four-(trimethyl silene ether) titaniums, other conditions be the same as Example 1.
Comparative example 6
The adsorbent product that the present invention is produced is added without, is adsorbed with activated carbon.
Embodiment 4
The hexachlorocyclotriph,sphazene crude product that purity is 99% is passed through and helped equipped with 500g embodiments 1-3 and comparative example the 1-6 purification made
In the 1000mL exchange columns of agent product, 80 DEG C of temperature, flow velocity 0.5BV/h, under the conditions of adsorb purification, flowed out with gas chromatographic detection
The weight/mass percentage composition of liquid, is shown in Table 1.
Table 1：Hexachlorocyclotriph,sphazene purity after the hexachlorocyclotriph,sphazene purification auxiliary agent absorption purification that different process is produced.
Claims (2)
1. a kind of hexachlorocyclotriph,sphazene purifies auxiliary agent, it is characterised in that including following material component：
Ingredients weight parts
Vinylidene 100
(Z) -3,7- dimethyl -2,6- octadienes -1- alcohol acetic esters 0.01-0.1
Carbon tetraene -2- ketone the 0.01-0.1 of 6,10,14,18- tetramethyls -5,9,13,17- 19
Ammonium persulfate 0.5-1.5
Polyvinyl alcohol 1.5-2.5
9- octadecene-1-ol phosphoesterase 30s .01-0.1
3- methyl isophthalic acids, 5- di-p-tolyl -1,4- pentaaza diene 0.1-0.5
Four-(trimethyl silene ether) titanium 0.5-1
Water 1000.
2. a kind of hexachlorocyclotriph,sphazene purifies the preparation method of auxiliary agent, it is characterised in that comprise the following steps：
A certain amount of vinylidene is distributed in water, the ratio according to claim 1 adds (Z) -3,7- dimethyl -2,6- pungent two
Alkene -1- alcohol acetic esters, GGA, ammonium persulfate and polyethylene
Alcohol, 9- octadecylene -1- alcohol phosphates, 3- methyl isophthalic acids, 5- di-p-tolyl-Isosorbide-5-Nitrae-pentaaza diene, four-(trimethyl silene
Ether) titanium, heating, at 80-100 DEG C, reaction 14-20 hours, product filtering, drying obtains hexachlorocyclotriph,sphazene purification and helps
Agent.
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