CN107903284A - The preparation method of hexaphenyl cyclotrisilazane - Google Patents
The preparation method of hexaphenyl cyclotrisilazane Download PDFInfo
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- CN107903284A CN107903284A CN201711433291.3A CN201711433291A CN107903284A CN 107903284 A CN107903284 A CN 107903284A CN 201711433291 A CN201711433291 A CN 201711433291A CN 107903284 A CN107903284 A CN 107903284A
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- hexaphenyl
- cyclotrisilazane
- ammonia
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- SHWQWXGIWFEYTA-UHFFFAOYSA-N 2,2,4,4,6,6-hexakis-phenyl-1,3,5,2,4,6-triazatrisilinane Chemical compound N1[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)N[Si](C=2C=CC=CC=2)(C=2C=CC=CC=2)N[Si]1(C=1C=CC=CC=1)C1=CC=CC=C1 SHWQWXGIWFEYTA-UHFFFAOYSA-N 0.000 title claims abstract description 103
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 103
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 48
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 42
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 21
- 239000000908 ammonium hydroxide Substances 0.000 claims abstract description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 13
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 230000006837 decompression Effects 0.000 claims abstract description 11
- 125000003963 dichloro group Chemical group Cl* 0.000 claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 11
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000000746 purification Methods 0.000 claims abstract description 10
- 229910000077 silane Inorganic materials 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000005292 vacuum distillation Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims description 12
- OGNSDRMLWYNUED-UHFFFAOYSA-N 1-cyclohexyl-4-[4-[4-(4-cyclohexylcyclohexyl)cyclohexyl]cyclohexyl]cyclohexane Chemical group C1CCCCC1C1CCC(C2CCC(CC2)C2CCC(CC2)C2CCC(CC2)C2CCCCC2)CC1 OGNSDRMLWYNUED-UHFFFAOYSA-N 0.000 claims description 11
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- UMVBXBACMIOFDO-UHFFFAOYSA-N [N].[Si] Chemical compound [N].[Si] UMVBXBACMIOFDO-UHFFFAOYSA-N 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- VDCSGNNYCFPWFK-UHFFFAOYSA-N diphenylsilane Chemical compound C=1C=CC=CC=1[SiH2]C1=CC=CC=C1 VDCSGNNYCFPWFK-UHFFFAOYSA-N 0.000 claims 1
- 239000007789 gas Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 18
- 238000013019 agitation Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 17
- -1 Hexaphenyl cyclotrisilazane Chemical compound 0.000 description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- DNVUQRLSJFZVBN-UHFFFAOYSA-N 1-phenyl-1,3,5,2,4,6-triazatrisilinane Chemical compound N1[SiH2]N[SiH2]N([SiH2]1)c1ccccc1 DNVUQRLSJFZVBN-UHFFFAOYSA-N 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- UGXMKSYKRKUMGY-UHFFFAOYSA-N 1,3,5,2,4,6-triazatrisilinane Chemical compound N1[SiH2]N[SiH2]N[SiH2]1 UGXMKSYKRKUMGY-UHFFFAOYSA-N 0.000 description 3
- 229910000062 azane Inorganic materials 0.000 description 3
- 235000010290 biphenyl Nutrition 0.000 description 3
- 239000004305 biphenyl Substances 0.000 description 3
- 125000006267 biphenyl group Chemical group 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- OSXYHAQZDCICNX-UHFFFAOYSA-N dichloro(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](Cl)(Cl)C1=CC=CC=C1 OSXYHAQZDCICNX-UHFFFAOYSA-N 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920002379 silicone rubber Polymers 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- MROCJMGDEKINLD-UHFFFAOYSA-N dichlorosilane Chemical compound Cl[SiH2]Cl MROCJMGDEKINLD-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010025 steaming Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000003944 tolyl group Chemical group 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
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/21—Cyclic compounds having at least one ring containing silicon, but no carbon in the ring
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses the preparation method of hexaphenyl cyclotrisilazane, comprise the following steps：1), the synthesis of hexaphenyl cyclotrisilazane：Using dichloro base silane as reaction raw materials, after solvent dissolves, ammonia is slowly introducing under agitation, when heat temperature raising reflux 7 10 is small, obtains the hexaphenyl cyclotrisilazane solution containing ammonium chloride impurities；2), the purification of hexaphenyl cyclotrisilazane：The hexaphenyl cyclotrisilazane solution that step 1) obtains is filtered while hot, filter residue is ammonium chloride, and filtrate decompression distillation, separates out hexaphenyl cyclotrisilazane, then filtering drying after vacuum distillation with ammonium hydroxide.Pass through the hexaphenyl cyclotrisilazane purity height of the method for the invention preparation, high income.
Description
Technical field
The present invention relates to the synthesis technical field of phenyl cyclosilazane, and in particular to the preparation side of hexaphenyl cyclotrisilazane
Method.
Background technology
Hexaphenyl cyclotrisilazane is one of important cyclosilazane, has larger space bit since it carries phenyl
Resistance, therefore its hydrolytic stability is very good, can be as the heat-resisting additive of silicon rubber, to improve silicon rubber oxide side chain
Crosslinking and the cyclisation of main chain are degraded, and can effectively improve the heat resistance of silicon rubber.Hexaphenyl cyclotrisilazane is long at 400 DEG C
Phase heats, and can take off phenyl generation three-dimensional polymer, be a kind of good heat-resisting paint.Therefore, hexaphenyl cyclotrisilazane
Preparation method is worth studying, and to obtain, purity is high, hexaphenyl cyclotrisilazane of high income
The content of the invention
It is an object of the invention to provide the preparation method of hexaphenyl cyclotrisilazane, prepared by the method for the invention
Hexaphenyl cyclotrisilazane purity is high, high income.
The present invention is achieved through the following technical solutions：
The preparation method of hexaphenyl cyclotrisilazane, comprises the following steps：
1), the synthesis of hexaphenyl cyclotrisilazane：Using dichloro base silane as reaction raw materials, after solvent dissolves,
Ammonia is slowly introducing under stirring condition, when heat temperature raising reflux 7-10 is small, obtains three silicon of hexaphenyl ring containing ammonium chloride impurities
Azane solution；
2), the purification of hexaphenyl cyclotrisilazane：The hexaphenyl cyclotrisilazane solution that step 1) obtains is filtered while hot,
Filter residue is ammonium chloride, and filtrate decompression distillation, separates out hexaphenyl cyclotrisilazane, then filtering drying after vacuum distillation with ammonium hydroxide.
Applicant is had found by long-term experiment：Six benzene can be prepared by being passed through ammonia into dichloro base silane
Base cyclotrisilazane.Meanwhile in the synthesis step of hexaphenyl cyclotrisilazane, the flow and stirring condition of ammonia are all to influence
The key factor of hexaphenyl cyclotrisilazane yield, specifically：1st, ammonia flow is excessive, and ammonia can take away a part of diphenyl two
Chlorination silicon raw material, causes yield to reduce；Flow is too small, causes energy consumption excessive.2nd, stir：If do not stirred, the chlorine of generation
Changing ammonium parcel raw material causes yield to decline.
The method that the hexaphenyl cyclotrisilazane solution that step 1) obtains directly is separated out after can directly cooling down with ammonium hydroxide, this
Method causes a large amount of losses of solvent (ammonium hydroxide), and the product purity after filtering is not high, and color is deeper.But in this hair
In bright, the present invention is filtered while hot by first, is filtered out ammonium chloride, can be avoided having substantial amounts of ammonium chloride during follow-up ammonia solvent,
Cause ammonium hydroxide to waste, meanwhile, it is capable to effectively avoid containing not dissolved ammonium chloride in hexaphenyl cyclotrisilazane, and then improve
The purity of hexaphenyl cyclotrisilazane, then hexaphenyl cyclotrisilazane is separated out with ammonium hydroxide after filtrate decompression is distilled, subtracted by liquid
The mode separated out after pressure distillation with ammonium hydroxide can not only ensure that hexaphenyl cyclotrisilazane will not lose, and ensure yield, Er Qieneng
Enough usage amounts for effectively lowering ammonium hydroxide.
Process of the invention by synthesizing hexaphenyl cyclotrisilazane using dichloro base silane and ammonia as reaction raw materials
In, rationally control the intake of ammonia and raw material is stirred, not only increase the yield of hexaphenyl cyclotrisilazane, and
Reaction rate is accelerated, meanwhile, the method for purification of hexaphenyl cyclotrisilazane is improved, by filtering hexaphenyl ring while hot
Three silazane solution, first remove ammonium chloride, and filtrate decompression distillation, hexaphenyl cyclotrisilazane is separated out after vacuum distillation with ammonium hydroxide,
The purity of hexaphenyl cyclotrisilazane can be effectively improved, in this way, three silicon of hexaphenyl ring prepared by the method for the invention
Azane has the advantages that purity height, high income.Use what invention the method prepared hexaphenyl cyclotrisilazane to say rate for 90%
Left and right, purity can reach 98% or so.
Further, mixing speed 80-85r/min.
In hexaphenyl cyclotrisilazane building-up process, it is particularly important that mixing speed, mixing speed is excessively slow, the chlorination of generation
Ammonium parcel raw material causes yield to decline, and mixing speed is too fast, and liquid splash, or even liquid can be caused to go out return duct.
Applicant is had found by long term test：Mixing speed is arranged to above range, hexaphenyl ring can be effectively improved
The yield of three silazane.
Further, being passed through for ammonia concretely comprises the following steps：Ammonia is slowly passed through on a small quantity before reflow, is to slowly warm up to back
After stream, ammonia flow is increased.
Solvent is in reflux state, portion of product can be prevented to be taken away by ammonia, and the reaction under reflux state is more abundant,
Most reactants react completely, can suitably increase ammonia flow.
Further, excess of ammonia gas is absorbed with water.
Further, the intake velocity of ammonia is 15L/h before reflux, and the intake velocity of preceding ammonia is 20L/h after reflux.
Applicant is had found by long-term experiment：Hexaphenyl cyclotrisilazane can be made by being set using above-mentioned intake velocity
Yield reaches highest.
Further, solvent is toluene.
Further, the weight ratio of solvent and dichloro base silane is 2.5-3:1.
The solvent of aforementioned proportion can not only realize being completely dissolved for dichloro base silane with dichloro base silane, and
And the waste of solvent can be avoided
Further, vacuum distillation concretely comprises the following steps：Filtrate decompression is poured into beaker when distilling to 1/3 and cooled down, then
Hexaphenyl cyclotrisilazane is separated out with ammonia solvent.
Further, the concentration of ammonium hydroxide is 10%.
Further, hexaphenyl cyclotrisilazane is separated out using excessive ammonia.
Ammonium hydroxide can excessively improve the speed of precipitation and reduce the number separated out, can reduce material and cost of labor, subtract
Few energy consumption, improves product quality.
Compared with prior art, the present invention have the following advantages and advantages：
Process of the invention by synthesizing hexaphenyl cyclotrisilazane using dichloro base silane and ammonia as reaction raw materials
In, rationally control the intake of ammonia and raw material is stirred, not only increase the yield of hexaphenyl cyclotrisilazane, and
Reaction rate is accelerated, meanwhile, the method for purification of hexaphenyl cyclotrisilazane is improved, by filtering hexaphenyl ring while hot
Three silazane solution, first remove ammonium chloride, and filtrate decompression distillation, hexaphenyl cyclotrisilazane is separated out after vacuum distillation with ammonium hydroxide,
The purity of hexaphenyl cyclotrisilazane can be effectively improved, in this way, three silicon of hexaphenyl ring prepared by the method for the invention
Azane has the advantages that purity height, high income.
Embodiment
For the object, technical solutions and advantages of the present invention are more clearly understood, with reference to embodiment, the present invention is made
Further to describe in detail, exemplary embodiment of the invention and its explanation are only used for explaining the present invention, are not intended as to this
The restriction of invention.
Embodiment 1：
The preparation method of hexaphenyl cyclotrisilazane, comprises the following steps：
1), the synthesis of hexaphenyl cyclotrisilazane：100ml toluene and 40g diphenyl are first added in 250ml three-necked flasks
Dichlorosilane, is passed through ammonia, and ammonia flow should not be too large, and the intake velocity of ammonia is 15L/h, is to slowly warm up to flow back, and increases
Ammonia flow, the intake velocity of ammonia is 20L/h, absorbs excess of ammonia gas with water, when reflux 7 is small, is obtained miscellaneous containing ammonium chloride
The hexaphenyl cyclotrisilazane solution of matter, the mixing speed are 80r/min；
2), the purification of hexaphenyl cyclotrisilazane：The hexaphenyl cyclotrisilazane solution that step 1) obtains is filtered while hot,
Filter residue is ammonium chloride, and filtrate decompression distillation, when steaming to 1/3, pours into beaker and cool down, then molten with excessive ammonia (concentration 10%)
Solution ammonium chloride simultaneously separates out hexaphenyl cyclotrisilazane, filters, and drying solid obtains 36g hexaphenyl cyclotrisilazanes.
In the present embodiment：It is 90% from diphenyl dichlorosilane to the yield of phenyl cyclotrisilazane.Meanwhile hexaphenyl
The purity of cyclotrisilazane is high.
Embodiment 2：
The preparation method of hexaphenyl cyclotrisilazane, comprises the following steps：
1), the synthesis of hexaphenyl cyclotrisilazane：120ml toluene and 40g diphenyl are first added in 250ml three-necked flasks
Dichlorosilane, is passed through ammonia, and ammonia flow should not be too large, and the intake velocity of ammonia is 15L/h, is to slowly warm up to flow back, and increases
Ammonia flow, the intake velocity of ammonia is 20L/h, absorbs excess of ammonia gas with water, when reflux 10 is small, is obtained miscellaneous containing ammonium chloride
The hexaphenyl cyclotrisilazane solution of matter, the mixing speed are 85r/min；
2), the purification of hexaphenyl cyclotrisilazane：The hexaphenyl cyclotrisilazane solution that step 1) obtains is filtered while hot,
Filter residue is ammonium chloride, and filtrate decompression distillation, when steaming to 1/3, pours into beaker and cool down, then molten with excessive ammonia (concentration 10%)
Solution ammonium chloride simultaneously separates out hexaphenyl cyclotrisilazane, filters, and drying solid obtains 36.5g hexaphenyl cyclotrisilazanes.
Comparative example 1：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the mistake of the synthesis of hexaphenyl cyclotrisilazane
Without stirring in journey, 26g hexaphenyl cyclotrisilazanes are finally obtained, i.e., yield is 65%, also, hexaphenyl cyclotrisilazane
Purity it is very low, prepared hexaphenyl cyclotrisilazane contains substantial amounts of diphenyl dichlorosilane.
Comparative example 2：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the mistake of the synthesis of hexaphenyl cyclotrisilazane
Mixing speed is 70r/min in journey, finally obtains 30g hexaphenyl cyclotrisilazanes, i.e., yield is 75%, also, hexaphenyl ring
The purity of three silazane is relatively low, and prepared hexaphenyl cyclotrisilazane contains the diphenyl dichlorosilane of part.
Comparative example 3：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the mistake of the synthesis of hexaphenyl cyclotrisilazane
Mixing speed is 90r/min in journey, finally obtains 32g hexaphenyl cyclotrisilazanes, i.e. yield is 80% (in whipping process liquid
Body, which splashes, causes yield to reduce), the purity of hexaphenyl cyclotrisilazane is higher.
Comparative example 4：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the mistake of the synthesis of hexaphenyl cyclotrisilazane
Cheng Zhong, the intake velocity of ammonia is always 100r/min, finally obtains 30g hexaphenyl cyclotrisilazanes, i.e. yield is 75%, six
The purity of phenyl cyclotrisilazane is higher.
Comparative example 5：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the mistake of the synthesis of hexaphenyl cyclotrisilazane
Cheng Zhong, the intake velocity of ammonia is always 110r/min, finally obtains 28g hexaphenyl cyclotrisilazanes, i.e. yield is 70%, six
The purity of phenyl cyclotrisilazane is higher.Comparative example 5：
Comparative example 6：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the mistake of the synthesis of hexaphenyl cyclotrisilazane
Cheng Zhong, the intake velocity of ammonia is always 120r/min, finally obtains 24g hexaphenyl cyclotrisilazanes, i.e. yield is 60%, six
The purity of phenyl cyclotrisilazane is higher.
Comparative example 7：
This comparative example is based on embodiment 1, with embodiment 1 difference lies in：In the purification process of hexaphenyl cyclotrisilazane
In：Hexaphenyl cyclotrisilazane solution is naturally cold go after directly with ammonium hydroxide separate out hexaphenyl cyclotrisilazane, finally obtain 38.5g
Hexaphenyl cyclotrisilazane, i.e. yield are 96%, and still, the purity of hexaphenyl cyclotrisilazane is relatively low, prepared hexaphenyl
Cyclotrisilazane contains substantial amounts of ammonium chloride.
From the Experimental Comparison of embodiment 1- embodiments 2 and comparative example 1- comparative examples 7：
1st, the yield of the hexaphenyl cyclotrisilazane prepared by the method for the invention is 90% or so, and purity
Height, single control ammonia intake velocity or control mixing speed can all influence the yield of hexaphenyl cyclotrisilazane, its
In, the intake velocity of ammonia also affects the purity of hexaphenyl cyclotrisilazane.
2nd, the yield of hexaphenyl cyclotrisilazane is reduced with the increase of ammonia intake velocity.
3rd, mixing speed is excessively slow, and the ammonium chloride parcel raw material of generation causes hexaphenyl cyclotrisilazane yield to decline, stirring
Excessive velocities, can cause liquid splash, or even liquid to go out return duct, also result under hexaphenyl cyclotrisilazane yield
Drop.
4th, the purity of hexaphenyl cyclotrisilazane can be improved by first filtering out the method for purification of ammonium chloride.
To sum up, the present invention as reaction raw materials using dichloro base silane and ammonia by synthesizing hexaphenyl cyclotrisilazane
During, rationally control the intake of ammonia and raw material be stirred, not only increase the yield of hexaphenyl cyclotrisilazane,
And reaction rate is accelerated, meanwhile, the method for purification of hexaphenyl cyclotrisilazane is improved, by filtering six benzene while hot
Base cyclotrisilazane solution, first removes ammonium chloride, filtrate decompression distillation, three silicon nitrogen of hexaphenyl ring is separated out after vacuum distillation with ammonium hydroxide
Alkane, can effectively improve the purity of hexaphenyl cyclotrisilazane, in this way, the hexaphenyl ring three prepared by the method for the invention
Silazane has the advantages that purity height, high income.
Above-described embodiment, has carried out the purpose of the present invention, technical solution and beneficial effect further
Describe in detail, it should be understood that the foregoing is merely the embodiment of the present invention, be not intended to limit the present invention
Protection domain, within the spirit and principles of the invention, any modification, equivalent substitution, improvement and etc. done, should all include
Within protection scope of the present invention.
Claims (10)
1. the preparation method of hexaphenyl cyclotrisilazane, it is characterised in that comprise the following steps：
1), the synthesis of hexaphenyl cyclotrisilazane：Using dichloro base silane as reaction raw materials, after solvent dissolves, stirring
Under the conditions of be slowly introducing ammonia, when heat temperature raising reflux 7-10 is small, obtain the hexaphenyl cyclotrisilazane containing ammonium chloride impurities
Solution；
2), the purification of hexaphenyl cyclotrisilazane：The hexaphenyl cyclotrisilazane solution that step 1) obtains is filtered while hot, filter residue
For ammonium chloride, filtrate decompression distillation, separates out hexaphenyl cyclotrisilazane, then filtering drying after vacuum distillation with ammonium hydroxide.
2. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that the mixing speed is
80-85r/min。
3. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that the ammonia is passed through
Concretely comprise the following steps：Ammonia is slowly passed through on a small quantity before reflow, after being to slowly warm up to reflux, increases ammonia flow.
4. the preparation method of hexaphenyl cyclotrisilazane according to claim 3, it is characterised in that excess of ammonia gas water
Absorb.
5. the preparation method of hexaphenyl cyclotrisilazane according to claim 3, it is characterised in that before reflux ammonia into
Gas velocity degree is 15L/h, and the intake velocity of preceding ammonia is 20L/h after reflux.
6. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that the solvent is first
Benzene.
7. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that the solvent and dichloro
The weight ratio of diphenyl silane is 2.5-3:1.
8. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that the vacuum distillation
Concretely comprise the following steps：Filtrate decompression is poured into beaker when distilling to 1/3 and cooled down, and then separates out three silicon nitrogen of hexaphenyl ring with ammonia solvent
Alkane.
9. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that the concentration of the ammonium hydroxide
For 10%.
10. the preparation method of hexaphenyl cyclotrisilazane according to claim 1, it is characterised in that using excessive ammonia
Separate out hexaphenyl cyclotrisilazane.
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| CN114507253A (en) * | 2022-01-20 | 2022-05-17 | 杭州四马化工科技有限公司 | Continuous production process of silazane |
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| CN112409800A (en) * | 2020-11-30 | 2021-02-26 | 北京宇航系统工程研究所 | Weather-resistant silicon nitrogen rubber with three-dimensional network structure and preparation method thereof |
| WO2022111288A1 (en) * | 2020-11-30 | 2022-06-02 | 北京宇航系统工程研究所 | Weather-resistant silazane rubber with three-dimensional network structure and preparation method therefor |
| CN114507253A (en) * | 2022-01-20 | 2022-05-17 | 杭州四马化工科技有限公司 | Continuous production process of silazane |
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