CN105384778B - The preparation method of fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound - Google Patents
The preparation method of fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound Download PDFInfo
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- CN105384778B CN105384778B CN201510707489.0A CN201510707489A CN105384778B CN 105384778 B CN105384778 B CN 105384778B CN 201510707489 A CN201510707489 A CN 201510707489A CN 105384778 B CN105384778 B CN 105384778B
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- methoxyl group
- alkyl
- silane
- methyl
- phosphorus heterocycle
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- -1 silane compound Chemical class 0.000 title claims abstract description 54
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 53
- 239000011574 phosphorus Substances 0.000 title claims abstract description 53
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 42
- 239000003063 flame retardant Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical class OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 107
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000005194 fractionation Methods 0.000 claims abstract description 30
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000006073 displacement reaction Methods 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 150000001875 compounds Chemical class 0.000 claims abstract description 6
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims abstract description 6
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 96
- 239000007788 liquid Substances 0.000 claims description 17
- 238000013517 stratification Methods 0.000 claims description 16
- 238000010792 warming Methods 0.000 claims description 16
- LZDKZFUFMNSQCJ-UHFFFAOYSA-N 1,2-diethoxyethane Chemical compound CCOCCOCC LZDKZFUFMNSQCJ-UHFFFAOYSA-N 0.000 claims description 9
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 claims description 6
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- SXPLZNMUBFBFIA-UHFFFAOYSA-N butyl(trimethoxy)silane Chemical compound CCCC[Si](OC)(OC)OC SXPLZNMUBFBFIA-UHFFFAOYSA-N 0.000 claims description 4
- MMLDMUBBKAHKOA-UHFFFAOYSA-N (5-ethyl-2-methyl-2-oxo-1,3,2$l^{5}-dioxaphosphinan-5-yl)methanol Chemical compound CCC1(CO)COP(C)(=O)OC1 MMLDMUBBKAHKOA-UHFFFAOYSA-N 0.000 claims 1
- 150000001934 cyclohexanes Chemical class 0.000 claims 1
- 230000006837 decompression Effects 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 229920000728 polyester Polymers 0.000 abstract description 5
- 239000003610 charcoal Substances 0.000 abstract description 4
- 239000003822 epoxy resin Substances 0.000 abstract description 3
- 229920000647 polyepoxide Polymers 0.000 abstract description 3
- 229920002635 polyurethane Polymers 0.000 abstract description 3
- 239000004814 polyurethane Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 3
- 239000011347 resin Substances 0.000 abstract description 3
- 229920000915 polyvinyl chloride Polymers 0.000 abstract description 2
- 239000004800 polyvinyl chloride Substances 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 2
- VXTFGYMINLXJPW-UHFFFAOYSA-N phosphinane Chemical compound C1CCPCC1 VXTFGYMINLXJPW-UHFFFAOYSA-N 0.000 abstract 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 84
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 23
- 229910052739 hydrogen Inorganic materials 0.000 description 23
- 239000001257 hydrogen Substances 0.000 description 23
- 239000000047 product Substances 0.000 description 20
- 229910052710 silicon Inorganic materials 0.000 description 20
- 239000010703 silicon Substances 0.000 description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 15
- 238000000354 decomposition reaction Methods 0.000 description 15
- 238000011084 recovery Methods 0.000 description 15
- 238000009835 boiling Methods 0.000 description 14
- 238000005292 vacuum distillation Methods 0.000 description 14
- 238000005406 washing Methods 0.000 description 13
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 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 class 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 description 8
- 239000001301 oxygen Substances 0.000 description 8
- 229910052760 oxygen Inorganic materials 0.000 description 8
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- ROSDSFDQCJNGOL-UHFFFAOYSA-N protonated dimethyl amine Natural products CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 6
- 239000000377 silicon dioxide Substances 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 239000005055 methyl trichlorosilane Substances 0.000 description 4
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-MICDWDOJSA-N Trichloro(2H)methane Chemical compound [2H]C(Cl)(Cl)Cl HEDRZPFGACZZDS-MICDWDOJSA-N 0.000 description 3
- AFCIMSXHQSIHQW-UHFFFAOYSA-N [O].[P] Chemical compound [O].[P] AFCIMSXHQSIHQW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- XYFCBTPGUUZFHI-UHFFFAOYSA-N phosphine group Chemical group P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-DYCDLGHISA-N Deuterium chloride Chemical compound [2H]Cl VEXZGXHMUGYJMC-DYCDLGHISA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 229910018540 Si C Inorganic materials 0.000 description 2
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 229940008099 dimethicone Drugs 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 150000002118 epoxides Chemical class 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- 229910010271 silicon carbide Inorganic materials 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- SAWKFRBJGLMMES-UHFFFAOYSA-N methylphosphine Chemical compound PC SAWKFRBJGLMMES-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C07F9/6571—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 oxygen atoms as the only ring hetero atoms
- C07F9/657163—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 oxygen atoms as the only ring hetero atoms the ring phosphorus atom being bound to at least one carbon atom
- C07F9/657181—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 oxygen atoms as the only ring hetero atoms the ring phosphorus atom being bound to at least one carbon atom the ring phosphorus atom and, at least, one ring oxygen atom being part of a (thio)phosphonic acid derivative
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5435—Silicon-containing compounds containing oxygen containing oxygen in a ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Molecular Biology (AREA)
- Fireproofing Substances (AREA)
Abstract
The present invention relates to a kind of preparation method of fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound, the structure of the compound is shown below：
Description
Technical field
The present invention relates to a kind of preparation method of fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound, tool
Body is related to a kind of fire retardant alkyl-dimethyl epoxide (1- oxygen -1- methyl -4- ethyl -1- phospha -2,6- dioxa-cyclohexyls -<4
>- methoxyl group) silane compound preparation method.The compound contains the dual ignition-proof element of phosphorus, silicon, and the collaboration of phosphorus silicon has higher
Flame-retarded efficiency, it is suitable as the fire-retardant of the materials such as polyester PBT, PET, polyurethane, unsaturated-resin, epoxy resin, polyvinyl chloride
Agent.
Background technology
With developing rapidly for science and technology, synthesis high polymer material is widely used, and is brought greatly to people's life
Easily simultaneously because its inflammability also brings great disaster hidden-trouble, this promotes the quick hair of fire-retardant science and technology
Exhibition.At present, the fire retardant that China produces and used is halogenated flame retardant mostly, and this based flame retardant can discharge substantial amounts of when burning
Smog and pernicious gas, cause secondary hazards.With the enhancing of the constantly improve and people's environmental consciousness of flame retardant regulation, halogen system resistance
The use of combustion agent is gradually restricted, thus promotes the fast development of halogen-free flame retardants.Wherein, the research of phosphorus flame retardant
Compare more, but traditional organophosphorous fire retardant still has the problems such as polarity is big, easy to migrate, electric property is poor；Silicon systems are fire-retardant
Agent is a kind of new halogen-free flame retardants, has the advantages that efficient, nontoxic, low cigarette, anti-drip, pollution-free, but due to price
The problems such as expensive, the development of silicon-series five-retardant is also set to receive certain limitation.
The invention discloses a kind of phosphorus, silicon synergistic flame retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound
Preparation method.The design of the compound is that the outstanding ignition-proof element of two kinds of phosphorus and silicon is embedded in same molecular structure, phosphorus silicon association
Same-action, flame-retarded efficiency is high, also prevents from producing melting drippage when material is heated；Preparing raw material methyl trimethoxy epoxide silicon
Alkane is the downstream product of the byproduct methyl trichlorosilane of industrial production dimethicone, solves methyl trichlorosilane for in-depth
Problem of complex utilization opens an effective way.
The content of the invention
It is an object of the invention to propose a kind of fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound
Preparation method, its preparation technology is simple, and equipment investment is few, and raw material is cheap and easy to get, and cost is cheap, does not produce three-waste pollution, can gram
Take deficiency of the prior art.
In order to realize foregoing invention purpose, present invention employs following technical scheme, alkyl-dimethyl epoxide (phosphorus as described above
Heterocycle methoxyl group) silane preparation method, it is characterised in that this method is：
In the reactor equipped with efficient fractionating device, the air in reactor, control 1- oxos -1- are fallen with nitrogen displacement
Methyl -4- ethyl -4- methylol -2,6- dioxa -1- phospha cyclohexanes are (referred to as：4- methylols -4- ethyls-Cyclic methyl phosphine
Acid esters) with the mol ratio of alkyl trimethoxysilane it is 1: 1-1: 1.4, organic solvent is added, is warming up to 80-130 DEG C, control
It is fractionated column top temperature and is not higher than 65 DEG C, distills out the methanol of generation, fractionation reaction 6-13h, produce, stop anti-until without methanol
Should, it is evaporated under reduced pressure and removes organic solvent (recovery uses), purified processing, obtains alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silicon
Alkane, the structure of the compound are shown below：
R=methyl, ethyl, propyl group or butyl in formula.
Alkyl trimethoxysilane as described above is MTMS, ethyl trimethoxy silane, propyl group three
Methoxy silane or butyl trimethoxy silane.
Organic solvent as described above is diethylene glycol dimethyl ether, ethylene glycol diethyl ether, dimethylformamide (DMF) or two
The ring of oxygen six, its dosage are that the volume milliliter number of organic solvent is 4- methylols -4- ethyls-Cyclic methyl phosphonate ester quality grams
2-4 times.
Purification treating method as described above is washed for the toluene added with product Theoretical Mass grams equal volume milliliter number
Wash, stratification, separate lower floor's feed liquid, then be evaporated under reduced pressure and remove a small amount of toluene and low boilers.
Alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane of the present invention is weak yellow liquid, be suitable as polyester PBT, PET,
The fire retardant of the materials such as polyurethane, unsaturated-resin, epoxy resin.
The preparation technology principle of alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane is shown below：
R=methyl, ethyl, propyl group or butyl in formula.
Compared with prior art, beneficial innovation of the invention is：
1. the preparation method of phosphorus of the present invention, silicon synergistic fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound
Novelty, contain C-P keys, C-Si keys and six-membered ring structure in product structure, these design features cause the compound physical
Stable performance is learned, decomposition temperature is high, and plasticity is good, good with high polymer material compatibility, adapts to add in the high temperature of engineering plastics
Work.
2. phosphorus of the present invention, silicon synergistic fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound contain phosphorus, silicon
Two kinds of ignition-proof elements, under high temperature, P elements are converted into phosphoric acid or polyphosphoric acid can be catalyzed the formation for facilitating charcoal, the polyphosphoric acid film of formation
There is heat-insulated anoxybiotic to act on；Silicon forms the silicon layer of charcoal of densification with carbon, the generation that can effectively prevent melting from dripping.Phosphorus, silicon are from different
Mechanism cooperative flame retardant, higher flame-retarded efficiency can be played.
3. phosphorus of the present invention, the raw materials used first of silicon synergistic fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound
Base trimethoxy silane is the accessory substance methyl trichlorosilane and methanol reaction gained by industrial production dimethicone, to solve
The pollution problem of methyl trichlorosilane opens an effective approach.
4. prepared by phosphorus of the present invention, silicon synergistic fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound compound
One esterification is more active, without adding catalyst, does not introduce impurity；Solvent and caused methanol in technique can be reclaimed directly
Use, do not cause three-waste pollution, be green preparation process.
It is 5. former used in the preparation of phosphorus of the present invention, silicon synergistic fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound
Expect cheap and easy to get, its technique is simple, and equipment investment is few, is easy to large-scale production, has application and DEVELOPMENT PROSPECT well.
Brief description of the drawings
In order to further illustrate that the structure of product and performance spy provide drawings described below.
Fig. 1 is the infrared spectrogram of methyl dimethoxy epoxide (phosphorus heterocycle methoxyl group) silane；Fig. 1 shows：2951cm-1With
2888cm-1(stretching vibration of c h bond)；1464cm-1And 1393cm-1(flexural vibrations of c h bond)；1267cm-1(P=O keys
Stretching vibration)；1186cm-1(stretching vibration of P-O keys)；1153cm-1(stretching vibration of Si-O keys) 1086cm-1And 1043cm-1
(the stretching vibration doublet of C-O keys)；851cm-1(stretching vibration of P-C keys).
Fig. 2 is the infrared spectrogram of ethyl dimethoxy (phosphorus heterocycle methoxyl group) silane；Fig. 2 shows：2963cm-1With
2893cm-1(stretching vibration of c h bond)；1458cm-1(flexural vibrations of c h bond)；1251cm-1(stretching vibration of P=O keys)；
1109cm-1(stretching vibration of Si-O-C keys)；832cm-1(flexural vibrations of Si-O-C keys)；990cm-1(P-O-C keys it is flexible
Vibration)；749cm-1(stretching vibration of Si-C keys).
Fig. 3 is the infrared spectrogram of dimethylamine epoxide (phosphorus heterocycle methoxyl group) silane；Fig. 3 shows：3000cm-1With
2872cm-1(stretching vibration of c h bond)；1442cm-1(flexural vibrations of c h bond)；1308cm-1(stretching vibration of P=O keys)；
1034cm-1(stretching vibration of Si-O-C keys)；878cm-1(flexural vibrations of Si-O-C keys)；950cm-1(P-O-C keys it is flexible
Vibration)；754cm-1(stretching vibration of Si-C keys).
Fig. 4 is the nuclear magnetic spectrum figure of methyl dimethoxy epoxide (phosphorus heterocycle methoxyl group) silane；Fig. 4 shows：Deuterochloroform is molten
Agent, δ 0.04-0.20 are Si-CH3The upper methyl hydrogen peak being connected with silicon；δ 0.81-0.86 are C-CH2CH3The methyl of upper and carbon phase even
Hydrogen peak；δ 1.20-1.35 are C-CH2CH3The methylene hydrogen peak of upper and carbon phase even；δ 1.50-1.62 are O=P-CH3Go up and phosphorus oxygen phase
Methyl hydrogen peak even；δ 3.97-4.18 are Si-OCH3The upper methyl hydrogen peak being connected with silica；δ 4.20-4.32 are Si-OCH2On C
The methylene hydrogen peak being connected with silica；δ 4.36-4.60 are (CH2O)2- P=O (- CH3) the methylene epoxide that is connected with oxygen on phosphine ring
Hydrogen peak；δ 7.26 is the proton peak that solvent carbon deuterium chloride exchanges.
Fig. 5 is the nuclear magnetic spectrum figure of ethyl dimethoxy (phosphorus heterocycle methoxyl group) silane；Fig. 5 shows：Deuterochloroform is molten
Agent, δ 0.69-0.76 are Si-CH2CH3The upper methylene hydrogen peak being connected with silicon；δ 0.77-0.86 are C-CH2CH3Upper and carbon phase connects
Methyl hydrogen peak；δ 1.08-1.17 are Si-CH2CH3The upper methyl hydrogen peak being connected with silicon；δ 1.19-1.34 are C-CH2CH3It is upper with
The methylene hydrogen peak of carbon phase even；δ 1.52-1.60 are O=P-CH3The upper methyl hydrogen peak being connected with phosphorus oxygen；δ 4.00-4.21 are Si-
OCH3The upper methyl hydrogen peak being connected with silica；δ 4.25-4.36 are Si-OCH2The upper methylene hydrogen peaks being connected with silica of C；δ4.43-
4.62 be (CH2O)2- P=O (- CH3) the methylene epoxide hydrogen peak that is connected with oxygen on phosphine ring；δ 7.26 is what solvent carbon deuterium chloride exchanged
Proton peak.
Fig. 6 is the nuclear magnetic spectrum figure of dimethylamine epoxide (phosphorus heterocycle methoxyl group) silane；Fig. 6 shows：Deuterochloroform is molten
Agent, δ 0.70-0.83 are Si-CH2CH2CH3The methylene hydrogen peak that upper and silicon is joined directly together；δ 0.84-0.92 are C-CH2CH3It is upper with
The methyl hydrogen peak of carbon phase even；δ 1.05-1.16 are Si-CH2CH2CH3The methyl hydrogen peak that upper and silicon is separated by；δ 1.16-1.31 are C-
CH2CH3The methylene hydrogen peak of upper and carbon phase even；δ 1.55-1.67 are Si-CH2CH2CH3The methylene hydrogen peak that upper and silicon is separated by；δ
1.67-1.81 it is O=P-CH3The upper methyl hydrogen peak being connected with phosphorus oxygen；δ 3.81-3.92 are Si-OCH3The upper first being connected with silica
Ji Qingfeng；δ 3.93-4.15 are Si-OCH2The upper methylene hydrogen peaks being connected with silica of C；δ 4.16-4.48 are (CH2O)2- P=O (-
CH3) the methylene epoxide hydrogen peak that is connected with oxygen on phosphine ring；δ 7.26 is the proton peak that solvent carbon deuterium chloride exchanges.
Embodiment
Technical scheme is described further below in conjunction with specific embodiment.
Embodiment 1 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 13.62g (0.10mol)
MTMS, 40ml diethylene glycol dimethyl ethers, 100 DEG C being warming up to, control fractionation column top temperature is not higher than 65 DEG C, point
The methanol of generation is distillated, reacts 8h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes diethylene glycol two
Methyl ether (recovery uses), then adds 30ml toluene agitator treating, is transferred to stratification in separatory funnel, separates lower layered material
Liquid, it is evaporated under reduced pressure and removes toluene and a small amount of low boilers, obtain methyl dimethoxy epoxide (phosphorus heterocycle methoxyl group) silane, product yield
95.5%, its flash-point (open cup)：204 ± 5 DEG C, decomposition temperature：248 ± 5 DEG C, density (25 DEG C)：1.679g/cm3, refractive power
Rate：nD 25=1.3842.
Embodiment 2 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 17.71g (0.13mol)
MTMS, 75ml ethylene glycol diethyl ethers, 80 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionation
The methanol being born, 11h is reacted, after being produced without methanol, make vacuum distillation apparatus into, be evaporated under reduced pressure and remove ethylene glycol diethyl ether
(recovery uses), 30ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid, depressurize
Toluene and a small amount of low boilers are distilled off, obtain methyl dimethoxy epoxide (phosphorus heterocycle methoxyl group) silane, product yield 90.6%, its
Flash-point (open cup)：204 ± 5 DEG C, decomposition temperature：248 ± 5 DEG C, density (25 DEG C)：1.679g/cm3, index of refraction：nD 25=
1.3842。
Embodiment 3 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 14.98g (0.11mol)
MTMS, 50mlDMF, 110 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionates out generation
Methanol, fractionation reaction 6h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes DMF (recovery uses), and
Add 30ml toluene washing afterwards, be transferred to stratification in separatory funnel, separate lower floor's feed liquid, be evaporated under reduced pressure remove toluene and
A small amount of low boilers, obtain methyl dimethoxy epoxide (phosphorus heterocycle methoxyl group) silane, product yield 86.5%, its flash-point (open cup)：
204 ± 5 DEG C, decomposition temperature：248 ± 5 DEG C, density (25 DEG C)：1.679g/cm3, index of refraction：nD 25=1.3842.
Embodiment 4 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 16.34g (0.12mol)
MTMS, 60ml dioxane, 90 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionation birth
Into methanol, react 10h, after being produced without methanol, make vacuum distillation apparatus into, be evaporated under reduced pressure and remove dioxane (recovery makes
With), 30ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid, be evaporated under reduced pressure and remove
Toluene and a small amount of low boilers, obtain methyl dimethoxy epoxide (phosphorus heterocycle methoxyl group) silane, product yield 93.4%, and its flash-point (is opened
Cup)：204 ± 5 DEG C, decomposition temperature：248 ± 5 DEG C, density (25 DEG C)：1.679g/cm3, index of refraction：nD 25=1.3842.
Embodiment 5 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 15.02g (0.10mol)
Ethyl trimethoxy silane, 40ml diethylene glycol dimethyl ethers, 110 DEG C being warming up to, control fractionation column top temperature is not higher than 65 DEG C, point
The methanol of generation is distillated, reacts 8h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes diethylene glycol two
Methyl ether (recovery uses), 32ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid,
It is evaporated under reduced pressure and removes toluene and a small amount of low boilers, obtains ethyl dimethoxy (phosphorus heterocycle methoxyl group) silane, product yield
84.5%, its flash-point (open cup)：200 ± 5 DEG C, decomposition temperature：253 ± 5 DEG C, density (25 DEG C)：1.680g/cm3, refractive power
Rate：nD 25=1.4027.
Embodiment 6 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 16.52g (0.11mol)
Ethyl trimethoxy silane, 55ml dioxane, 90 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionation birth
Into methanol, react 13h, after being produced without methanol, make vacuum distillation apparatus into, be evaporated under reduced pressure and remove dioxane (recovery makes
With), 32ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid, be evaporated under reduced pressure and remove
Toluene and a small amount of low boilers, obtain ethyl dimethoxy (phosphorus heterocycle methoxyl group) silane, product yield 85.5%, and its flash-point (is opened
Cup)：200 ± 5 DEG C, decomposition temperature：253 ± 5 DEG C, density (25 DEG C)：1.680g/cm3, index of refraction：nD 25=1.4027.
Embodiment 7 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 18.02g (0.12mol)
Ethyl trimethoxy silane, 60mlDMF, 100 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionates out generation
Methanol, fractionation reaction 10h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes DMF (recovery uses), and
Add 32ml toluene washing afterwards, be transferred to stratification in separatory funnel, separate lower floor's feed liquid, be evaporated under reduced pressure remove toluene and
A small amount of low boilers, obtain ethyl dimethoxy (phosphorus heterocycle methoxyl group) silane, product yield 88.0%, its flash-point (open cup)：
200 ± 5 DEG C, decomposition temperature：253 ± 5 DEG C, density (25 DEG C)：1.680g/cm3, index of refraction：nD 25=1.4027.
Embodiment 8 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 19.53g (0.13mol)
Ethyl trimethoxy silane, 45ml ethylene glycol diethyl ethers, 120 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionation
The methanol being born, fractionation reaction 6h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes ethylene glycol two
Ether (recovery uses), 32ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid,
It is evaporated under reduced pressure and removes toluene and a small amount of low boilers, obtains ethyl dimethoxy (phosphorus heterocycle methoxyl group) silane, product yield
95.8%, its flash-point (open cup)：200 ± 5 DEG C, decomposition temperature：253 ± 5 DEG C, density (25 DEG C)：1.680g/cm3, refractive power
Rate：nD 25=1.4027.
Embodiment 9 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 18.07g (0.11mol)
Propyl trimethoxy silicane, 50ml diethylene glycol dimethyl ethers, 110 DEG C being warming up to, control fractionation column top temperature is not higher than 65 DEG C, point
The methanol of generation is distillated, reacts 10h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes diethylene glycol two
Methyl ether (recovery uses), 33ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid,
It is evaporated under reduced pressure and removes toluene and a small amount of low boilers, obtains dimethylamine epoxide (phosphorus heterocycle methoxyl group) silane, product yield
86.5%, its flash-point (open cup)：206 ± 5 DEG C, decomposition temperature：258 ± 5 DEG C, density (25 DEG C)：1.692g/cm3, refractive power
Rate：nD 25=1.4239.
Embodiment 10 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 23.00g (0.14mol)
Propyl trimethoxy silicane, 60mlDMF, 120 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionates out generation
Methanol, fractionation reaction 8h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes DMF (recovery uses), and
Add 33ml toluene washing afterwards, be transferred to stratification in separatory funnel, separate lower floor's feed liquid, be evaporated under reduced pressure remove toluene and
A small amount of low boilers, obtain dimethylamine epoxide (phosphorus heterocycle methoxyl group) silane, product yield 89.2%, its flash-point (open cup)：
206 ± 5 DEG C, decomposition temperature：258 ± 5 DEG C, density (25 DEG C)：1.692g/cm3, index of refraction：nD 25=1.4239.
Embodiment 11 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 19.72g (0.12mol)
Propyl trimethoxy silicane, 50ml dioxane, 90 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionation birth
Into methanol, react 11h, after being produced without methanol, make vacuum distillation apparatus into, be evaporated under reduced pressure and remove dioxane (recovery makes
With), 33ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid, be evaporated under reduced pressure and remove
Toluene and a small amount of low boilers, obtain dimethylamine epoxide (phosphorus heterocycle methoxyl group) silane, product yield 94.7%, and its flash-point (is opened
Cup)：206 ± 5 DEG C, decomposition temperature：258 ± 5 DEG C, density (25 DEG C)：1.692g/cm3, index of refraction：nD 25=1.4239.
Embodiment 12 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 21.36g (0.13mol)
Propyl trimethoxy silicane, 40ml ethylene glycol diethyl ethers, 130 DEG C being warming up to, control fractionation column top temperature is not higher than 65 DEG C, point
The methanol of generation is distillated, fractionation reaction 6h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes ethylene glycol
Diethyl ether (recovery uses), 33ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower layered material
Liquid, it is evaporated under reduced pressure and removes toluene and a small amount of low boilers, obtain dimethylamine epoxide (phosphorus heterocycle methoxyl group) silane, product yield
87.6%, its flash-point (open cup)：206 ± 5 DEG C, decomposition temperature：258 ± 5 DEG C, density (25 DEG C)：1.692g/cm3, refractive power
Rate：nD 25=1.4239.
Embodiment 13 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 21.40g (0.12mol)
Butyl trimethoxy silane, 60ml diethylene glycol dimethyl ethers, 130 DEG C being warming up to, control fractionation column top temperature is not higher than 65 DEG C, point
The methanol of generation is distillated, reacts 6h, after being produced without methanol, makes vacuum distillation apparatus into, is evaporated under reduced pressure and removes diethylene glycol two
Methyl ether (recovery uses), 35ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid,
It is evaporated under reduced pressure and removes toluene and a small amount of low boilers, obtains butyl dimethoxy (phosphorus heterocycle methoxyl group) silane, product yield
83.0%, its flash-point (open cup)：207 ± 5 DEG C, decomposition temperature：265 ± 5 DEG C, density (25 DEG C)：1.703g/cm3, refractive power
Rate：nD 25=1.4683.
Embodiment 14 equipped with agitator, thermometer, efficient fractionating device 150ml four-hole boiling flasks in, use nitrogen displacement
Air in bottle falling, add 19.40g (0.10mol) 4- methylols -4- ethyls-Cyclic methyl phosphonate ester, 24.96g (0.14mol)
Butyl trimethoxy silane, 50ml ethylene glycol diethyl ethers, 120 DEG C are warming up to, control fractionation column top temperature is not higher than 65 DEG C, fractionation
The methanol being born, 10h is reacted, after being produced without methanol, make vacuum distillation apparatus into, be evaporated under reduced pressure and remove ethylene glycol diethyl ether
(recovery uses), 35ml toluene washing is then added, stratification in separatory funnel is transferred to, separates lower floor's feed liquid, depressurize
Toluene and a small amount of low boilers are distilled off, obtain butyl dimethoxy (phosphorus heterocycle methoxyl group) silane, product yield 92.8%, its
Flash-point (open cup)：207 ± 5 DEG C, decomposition temperature：265 ± 5 DEG C, density (25 DEG C)： 1.703g/cm3, index of refraction：nD 25=
1.4683。
The preparation example main technologic parameters of table 1
Alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane of above-mentioned preparation is also applied to polyester PBT by inventor
In.Reference：GB/T2406-2008《Plastics Combustion method for testing performance-oxygen index method》The limited oxygen index of test sample product.Take product
After alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane and polyester PBT are well mixed in varing proportions, are extruded, be made with extruder
A diameter of 3mm batten, and its fire resistance is tested, result of the test is as shown in the table：
The alkyl-dimethyl epoxide of table 2 (phosphorus heterocycle methoxyl group) silane is applied to PBT fire resistance data
As can be seen from Table 2 when fire retardant addition of the present invention is up to 25%, the equal energy of limited oxygen index of flame-retardant PBT system
Reach 28% or more, be provided with good flame retardant effect, and the defects of dripping easily has been melted in heated or burning to it
Improve.Therefore, fire retardant of the present invention has good fire resistance and into charcoal anti-drip energy.
Claims (2)
1. a kind of preparation method of fire retardant alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound, it is characterised in that should
Method is：
In the reactor equipped with fractionating device, the air in reactor, control 1- oxo -1- methyl -4- are fallen with nitrogen displacement
The mol ratio of ethyl -4- methylols -2,6- dioxa -1- phospha cyclohexanes and alkyl trimethoxysilane is 1: 1-1: 1.4, then
Add 2-4 times of volume of 1- oxo -1- methyl -4- ethyl -4- methylol -2,6- dioxa -1- phospha cyclohexane quality grams
The diethylene glycol dimethyl ether or ethylene glycol diethyl ether of milliliter number are warming up to 80-130 DEG C, control fractionation capital as organic solvent
Temperature is not higher than 65 DEG C, distills out the methanol of generation, fractionation reaction 6-13h, is produced until without methanol, stop reaction, decompression is steamed
Organic solvent is removed in distillation, adds and is washed with the toluene of product Theoretical Mass grams equal volume milliliter number, stratification, is separated down
Layered material liquid, then be evaporated under reduced pressure and remove a small amount of toluene and low boilers, alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane is obtained, should
The structure of compound is shown below：
R=methyl, ethyl, propyl group or butyl in formula.
2. the preparation method of alkyl-dimethyl epoxide (phosphorus heterocycle methoxyl group) silane compound as claimed in claim 1, its feature exist
In：Described alkyl trimethoxysilane is MTMS, ethyl trimethoxy silane, propyl trimethoxy silicane
Or butyl trimethoxy silane.
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