CN110483776A - A kind of synthetic method and its synthesizer of high purity silicone oil - Google Patents
A kind of synthetic method and its synthesizer of high purity silicone oil Download PDFInfo
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- CN110483776A CN110483776A CN201910797498.1A CN201910797498A CN110483776A CN 110483776 A CN110483776 A CN 110483776A CN 201910797498 A CN201910797498 A CN 201910797498A CN 110483776 A CN110483776 A CN 110483776A
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- silicone oil
- high purity
- catalyst
- synthetic method
- azeotropic
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- 229920002545 silicone oil Polymers 0.000 title claims abstract description 73
- 238000010189 synthetic method Methods 0.000 title claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 57
- -1 polysiloxanes ring Polymers 0.000 claims abstract description 40
- 239000002904 solvent Substances 0.000 claims abstract description 35
- 239000003054 catalyst Substances 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 32
- 238000009835 boiling Methods 0.000 claims abstract description 22
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 17
- 239000000376 reactant Substances 0.000 claims abstract description 11
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 10
- 238000012545 processing Methods 0.000 claims abstract description 10
- 238000004519 manufacturing process Methods 0.000 claims abstract description 6
- 238000004064 recycling Methods 0.000 claims description 52
- 238000010438 heat treatment Methods 0.000 claims description 21
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 13
- 230000018044 dehydration Effects 0.000 claims description 7
- 238000006297 dehydration reaction Methods 0.000 claims description 7
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 6
- BKIMMITUMNQMOS-UHFFFAOYSA-N nonane Chemical compound CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 claims description 6
- 230000006837 decompression Effects 0.000 claims description 5
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 3
- 239000011949 solid catalyst Substances 0.000 claims description 3
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 claims description 2
- ISYGDEPVQGOIRI-UHFFFAOYSA-N [SiH3]O[SiH3].CC=C Chemical compound [SiH3]O[SiH3].CC=C ISYGDEPVQGOIRI-UHFFFAOYSA-N 0.000 claims description 2
- 229940008099 dimethicone Drugs 0.000 claims description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 125000003944 tolyl group Chemical group 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 20
- 239000000126 substance Substances 0.000 abstract description 15
- 238000009833 condensation Methods 0.000 abstract description 5
- 230000005494 condensation Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 29
- 150000003384 small molecules Chemical group 0.000 description 15
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical group [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 14
- 229920001296 polysiloxane Polymers 0.000 description 11
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 229920001610 polycaprolactone Polymers 0.000 description 9
- 239000004632 polycaprolactone Substances 0.000 description 9
- 229910052710 silicon Inorganic materials 0.000 description 9
- 239000010703 silicon Substances 0.000 description 9
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 8
- 238000010792 warming Methods 0.000 description 8
- 239000003513 alkali Substances 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000003292 glue Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 5
- 230000008676 import Effects 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 239000000470 constituent Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 4
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000009834 vaporization Methods 0.000 description 4
- 230000008016 vaporization Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000008364 bulk solution Substances 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000199 molecular distillation Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N vinyl-ethylene Natural products C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Natural products P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Silicon Polymers (AREA)
Abstract
The invention belongs to the technical field of chemical materials more particularly to the synthetic methods and its synthesizer of a kind of high purity silicone oil.The present invention provides a kind of synthetic methods of high purity silicone oil, include the following steps step 1, polysiloxanes ring body, end-capping reagent and catalyst are mixed and reacted, obtain reactant 1；Step 2 after removing the catalyst of the reactant 1, obtains product 1；Step 3 mixes the product 1 with azeotropic solvent, carries out azeotropic processing, obtains high purity silicone oil.The present invention is by introducing a kind of low-boiling organic alkane azeotropic solvent into silicone oil synthetic reaction system, cooperate azeotropic and condensation process, provide a kind of efficient, easy, low-cost silicone oil method of purification and production technology, obtained silicone oil purity is high, can meet different industries to the particular/special requirement of silicone oil quality.
Description
Technical field
The invention belongs to the technical field of chemical materials more particularly to the synthetic methods and its synthesis of a kind of high purity silicone oil
Device.
Background technique
Silicone oil has in every profession and trades such as medical treatment, food, electric power, automobile, industry and largely answers as a kind of basic material
With, while silicone oil is also the base polymer for preparing various organic silicon rubber products.
Silicone oil main component is polysiloxane, and synthesis is to make using cyclic organic siloxane as raw material in acid or alkali
Linear polyorganosiloxane is made by ring-opening polymerisation under catalysts conditions.Because of the ring-opening polymerization of cyclic organic siloxane,
It is an equilibration reaction, there is the annular siloxane of 12-14% or so, including three silicon of pregnancy basic ring always in synthetic reaction
The small molecule ring body of the D3-D20 such as oxygen alkane (D3), octamethylcy-clotetrasiloxane (D4), decamethylcyclopentaandoxane (D5), there is also
The poly- organic oxygen alkane of a small amount of small molecule linear body.In general, silicone oil synthesis passes through the method for heating decompression after the completion of balanced reaction
Deviate from small molecule, it is general that reaction kettle is used to blast the abjection that the inert gases such as nitrogen promote small molecule to improve silicone oil purity, or
Person uses thin film evaporation container, molecular distillation container, and reaction system is removed small point by heating reduced pressure treatment by the methods of extraction
Sub- polysiloxanes.But the existing synthetic method for improving silicone oil purity still has the technology that can not remove small molecule completely
Defect.If the synthetic reaction of silicone oil usually carries out in vertical response kettle, in reaction kettle, the additive amount maximum of liquid, which is no more than, holds
Long-pending 2/3rds, and level is higher, and low molecular content boiling point all with higher in silicone oil, as the boiling point of D3 is
134 DEG C, the boiling point of D4 is 175 DEG C, and the boiling point of D5 is 210 DEG C, and with the increase of molecular weight, boiling point is also higher and higher, due to silicon
The heatproof limitation of oil, reaction kettle material heating temperature is generally at 200 DEG C or so.When decompression takes off low, due to reaction kettle upper layer three
/ mono- space, easily formation temperature are poor, cause the low molecular weight polycaprolactone siloxanes of vaporization to be constantly condensed back, can not take off completely
Out.And the method that the inert gases such as nitrogen are blasted using reactor bottom, the low molecular weight polycaprolactone siloxanes of vaporization is taken out of, because of gas
The dispersion degree of bulging bubble is not enough, and is easily assembled, and it is limited to take low molecular weight polycaprolactone siloxanes amount out of, and presence can not recycle, at
The problems such as this height, the time is long, and tail gas easily causes environmental pollution.And the methods of thin film evaporation container or molecular distillation container are used,
Complex process, equipment is expensive, and mass production is at high cost etc..And addition methanol, ethyl alcohol, the extraction of acetic acid equal solvent is used to separate again
The method of distillation, because the principle of extraction is the extractant selected and the bulk solution that is extracted is immiscible and bulk solution
In impurity mix, but low molecular weight polycaprolactone siloxanes ring body itself is identical as silicone oil component, selects methanol, ethyl alcohol, acetic acid etc. molten
Agent is incompatible with silicone oil main body, also limited with the compatibility of low molecular weight polycaprolactone siloxanes, and time-consuming for extraction, is unable to reach ideal effect
Fruit.Therefore, the small molecule polysiloxane level that above method removes is limited, so in commercially available routine silicone product standard,
Its fugitive constituent indication range is generally 1%-3%.
Since lower-molecular substance remaining in silicone oil can occur to volatilize and ooze out in long-term use, electronics electricity is easily caused
Contact fault in the products such as device, surface optical device is smudgy, in electrical insulation properties decline and the industries such as food, medical treatment
The problems such as hazardous substance content is exceeded.Therefore, develop a kind of high purity silicone oil synthetic method be those skilled in the art urgently
The technical issues of solution.
Summary of the invention
In view of this, the purpose of the present invention is develop a kind of synthetic method of simple, the high-efficient high purity silicone oil of method.
The present invention provides a kind of synthetic methods of high purity silicone oil, comprising the following steps:
Polysiloxanes ring body, end-capping reagent and catalyst are mixed and are reacted by step 1, obtain reactant 1；
Step 2 after removing the catalyst of the reactant 1, obtains product 1；
Step 3 mixes the product 1 with azeotropic solvent, carries out azeotropic processing, obtains high purity silicone oil.
Specifically, the polysiloxanes ring body is 100 parts by weight, the end-capping reagent is 0.1-5 parts by weight, the catalyst
It is 5-200 parts by weight for 0.01-3 parts by weight and the azeotropic solvent.
Preferably, the polysiloxanes ring body is selected from dimethicone, methylvinylcyclosiloxane, methylbenzene
One of cyclosiloxane, hexichol cyclosiloxane, methyl trifluoro propyl cyclosiloxane and methylhydracyclosiloxane are a variety of.
Preferably, the end-capping reagent is selected from two silicon of hexamethyldisiloxane, methyl ethylene disiloxane and methyl hydrogen
One of oxygen alkane is a variety of.
Preferably, the catalyst is selected from acidic catalyst, basic catalyst or solid catalyst.
Preferably, the basic catalyst is selected from tetramethylammonium hydroxide or/and potassium hydroxide；
The solid catalyst is selected from resin cation or/and linear polychloride phosphine nitrile；
The acidic catalyst is selected from phosphoric acid or/and hydrochloric acid.
Specifically, after mixing polysiloxanes ring body, end-capping reagent and catalyst, can heat and be reacted in step 1,
The temperature of heating is 100-130 DEG C.Preferably, the temperature of heating is 105-115 DEG C.
Preferably, the azeotropic solvent is boiling point in 200 DEG C of organic alkanes below.
Preferably, the azeotropic solvent is selected from one of pentane, hexane, heptane, octane and nonane or a variety of.
Preferably, the weight ratio of the azeotropic solvent and the product 1 is (5-200): 100.
Preferably, including: in step 1
Step 1a, decompression dehydration processing will be carried out after the heating of polysiloxanes ring body, obtains product one；
Step 1b, the product one is reacted with end-capping reagent and catalyst Hybrid Heating, obtains reactant 1.
Specifically, the heating temperature of the polysiloxanes ring body heating is 60-80 DEG C, the decompression dehydration in step 1a
Time is 10~60min；
In step 1b, 100-130 DEG C of heating temperature by the product one and end-capping reagent and catalyst Hybrid Heating,
The heating time is 1-4h, specifically, in step 1b, the product one is carried out with end-capping reagent and catalyst Hybrid Heating flat
Weighing apparatus reaction, it is preferred that the heating temperature by the product one and end-capping reagent and catalyst Hybrid Heating is 105-115 DEG C.
Specifically, the heating temperature of the polysiloxanes ring body heating is 60-80 DEG C, wherein 60-80 DEG C in step 1a
It is dehydration temperaturre early period, for dehydration temperaturre early period for adding end-capping reagent and catalyst reaction not yet, not reaction temperature, described to subtract
The press-dehydrating time can also be subject to frozen-free object abjection.
Present invention also provides the synthesizers of the high purity silicone oil described in one kind, comprising:
Reaction kettle, horizontal rotary evaporator, condenser and recycling can；
The reaction kettle is connect with the horizontal rotary evaporator pipeline, and the bottom of the horizontal-type evaporator goes out equipped with silicone oil
Mouthful, the top of the horizontal rotary evaporator is equipped with material inlet；
The horizontal rotary evaporator is connect with the condenser tubes；
The condenser is connect with the recycling can pipeline.
It is reacted specifically, reaction kettle is used to mix polysiloxanes ring body, end-capping reagent and catalyst, obtains reactant
Behind 1, and catalyst for removing the reactant 1, product 1 is obtained.
Specifically, horizontal rotary evaporator carries out azeotropic processing for mixing the product 1 with azeotropic solvent.
Specifically, condenser is used to that azeotropic will to be carried out in horizontal rotary evaporator to condense with the steam generated.
Specifically, recycling can is for collecting the condensed azeotropic solvent of condenser and small-molecule substance.
Specifically, recycling can includes the first sub- recycling can and the second sub- recycling can, condenser passes through triple valve and the first son
Recycling can and the second sub- recycling can connection, the first sub- recycling can is for recycling azeotropic solvent, and the second sub- recycling can is for recycling D3-
D20 small-molecule substance.
Specifically, using the application synthesizer when, polysiloxanes ring body, end-capping reagent and catalyst can individually be thrown
Into in reaction kettle, reaction kettle can be the reactor of the temperature-adjustable capable of stirring equipped with motor, after individually feeding intake, poly- silicon oxygen
Alkane ring body, end-capping reagent and catalyst can be hybrid reaction in reaction kettle；Polysiloxanes ring body, end-capping reagent and catalyst can also be with
It after being pre-mixed, knocks down in reaction kettle and is reacted, reaction kettle may be the reactor with temperature-adjustable；Reaction terminates
Afterwards, catalyst can by high temperature, in and/or filtration treatment remove, then product 1 is conveyed into horizontal rotary evaporator, will be total to
Boil-off dose is added from the import of horizontal rotary evaporator, is then carried out azeotropic processing, is obtained high purity silicone oil, while azeotropic being produced
Raw steam is conveyed into condenser, and the azeotropic solvent of different boiling and D3-D20 small-molecule substance enter back through pipeline after condensation
Cycling and reutilization in closed cans.
Present invention also provides the synthesizers of the high purity silicone oil described in one kind to be equipped with reaction kettle, horizontal rotary evaporates
Device, condenser and recycling can, by reacting raw material in a kettle, by product and azeotropic solvent in horizontal rotary evaporator
Azeotropic processing is carried out, obtains the silicone oil of high-purity, and by the way that condenser and recycling can is arranged by azeotropic solvent condensing recovery, then benefit
With.The silicone oil product purity that synthetic method of the invention obtains is tested through gas-chromatography (GC) method and volatilization, volatilizable small
Molecule content is less than 0.5%wt.
Preferably, the horizontal rotary evaporator is long greater than high rotary evaporator.
Preferably, step 2 specifically includes: by high temperature, in and/or filtration treatment remove the catalyst of the reactant 1
Afterwards, product 1 is obtained.
Preferably, being specifically included in step 3: the product 1 and the azeotropic solvent in horizontal rotary evaporator into
The processing of row azeotropic, obtains high purity silicone oil.
It should be noted that the horizontal rotary evaporator is long greater than high rotary evaporator.
Specifically, specifically including in step 3: the product 1 in horizontal rotary evaporator, is taken out true with the azeotropic solvent
Empty extremely -0.06MPa is hereinafter, progress azeotropic processing, obtains high purity silicone oil.
More preferably, the azeotropic temperature is 25-200 DEG C in step 3.
Azeotropic temperature range is 25-200 DEG C.Because of the difference according to selection azeotropic solvent boiling point, the temperature that azeotropic starts
Can be different, azeotropic solvent can be one of pentane, hexane, heptane, octane and nonane or a variety of, such as n-hexane is just
Standard atmospheric pressure boiling point is 60 DEG C or so, just has azeotropic solution steaming for 40 DEG C or so when being decompressed to -0.06MPa or less distillation
Out, selection azeotropic solvent boiling point is lower, and the boiling point that azeotropic starts will be lower, constantly has difference altogether as temperature gradually rises
The liquid of boiling point steams, until 200 DEG C of low molecular substances have been deviate from substantially completely, so azeotropic temperature is preferably 25-200 DEG C.
It should be noted that azeotropic solvent deviates from polysiloxanes small molecule, by the azeotropic solvent and polysiloxanes after vaporization
Small molecule accesses different solvents by triple valve after shell and tube condenser condenses, by the condensed fluid under different temperatures, realizes
The separation and recovery of azeotropic solvent and polysiloxanes small molecule, therefore, high purity silicon after being evaporated in horizontal rotary evaporator
Oil product.
The present invention is directed to overcome the prior art that can not prepare the technical deficiency of high purity silicone oil, a kind of high purity silicon is provided
The synthetic method and production technology of oil: a kind of compare low molecule by introducing into the polyorganosiloxane mixtures after balanced reaction
The big organic alkane of polysiloxanes low boiling point, boiling point difference reduces azeotropic using organic alkane and low molecular weight polycaprolactone siloxanes azeotropic
Object boiling point and vapourizing temperature, while horizontal rotary evaporator is used, upper space volume is reduced, is substantially reduced because of upper space temperature
It is condensed back caused by difference and polysiloxanes boiling point are high.The present invention is by the way of liquid azeotropic, azeotropic solvent and polysiloxanes
Mixture mixes more abundant, the organic alkane constantly largely vaporized, can sufficiently take low molecular weight polycaprolactone siloxanes out of.It is organic after vaporization
Alkane is condensed through shell and tube condenser, with low molecular weight polycaprolactone siloxanes boiling point difference is directly separated and is recycled using organic alkane and is organic
Alkane and low molecular weight polycaprolactone siloxanes, recycling.The method and technique reduce the production procedure of silicone oil significantly, improve efficiency, together
When obtain silicone oil purity is high, volatile content is extremely low, can meet different industries to the particular/special requirement of silicone oil quality.Of the invention
The silicone oil product purity that synthetic method obtains is tested through gas-chromatography (GC) method and volatilization, and volatilizable small molecule content is less than
0.5%wt.It is compared with the traditional method, the technical solution of the application introduces azeotropic solvent, in addition, cooperating conjunction provided by the present application
At device, it is easier to recycling design and the production efficiency for improving silicone oil.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described.
Fig. 1 shows the synthesizer of high purity silicone oil provided by the invention；
Wherein, appended drawing reference, reaction kettle 1, reaction kettle outlet 1-1, horizontal rotary evaporator 2, horizontal rotary evaporator into
Mouth 2-1, the 4th material inlet 2-2, horizontal rotary evaporator outlet 2-3, high purity silicon oil export 2-4, condenser 3, condenser
Import 3-1, condensator outlet 3-2, triple valve 7, the second sub- recycling can 4, the second sub- recycling can import 4-1, the first sub- recycling can
5, the first sub- recycling can import 5-1, motor 6, the first material inlet A, the second material inlet B, third material inlet C, the 4th original
Expect D, silicone oil finished product E.
Specific embodiment
The present invention provides a kind of synthetic method of high purity silicone oil and its synthesizers, for solving prior art synthesis
Silicone oil purity it is low, the technological deficiency of lower-molecular substance can not be completely removed.
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Wherein, it is commercially available or self-control that following embodiment is raw materials used.
Embodiment 1
The embodiment of the present invention provides the first synthetic method of high purity silicone oil, specifically:
As shown in Figure 1, the embodiment of the invention provides the synthesizers of high purity silicone oil, comprising: reaction kettle 1, horizontal rotation
Turn evaporator 2, condenser 3, triple valve 7, the second sub- recycling can 4, the first sub- recycling can 5；Reaction kettle exports 1-1 and horizontal rotary
Evaporator 2-1 is connected by pipeline, and the bottom of horizontal rotary evaporator 2 is equipped with high purity silicon oil export 2-4, horizontal rotary
The top of evaporator 2 is equipped with the 4th material inlet 2-2；Horizontal rotary evaporator outlet 2-3 and condenser inlet 3-1 pass through pipeline
Connection；Condensator outlet 3-2 is connect with the second sub- recycling can 4 and the first sub- 5 pipeline of recycling can respectively by triple valve 7.
In the synthesizer of the high purity silicone oil of the embodiment of the present invention, by the octamethylcy-clotetrasiloxane of 100 parts by weight
It is knocked down in reaction kettle 1 by the first material inlet A, is warming up to 60 DEG C, open vacuum to -0.06MPa hereinafter, dehydration 30 minutes,
The tetramethylammonium hydroxide alkali glue of the tetramethyl divinyl siloxanes closure agent of 2 parts by weight and 0.02 parts by weight is passed through respectively
Second material inlet B and third material inlet C are knocked down in reaction kettle 1, are warming up to balanced reaction 4 hours at 105-115 DEG C, reaction
Tetramethylammonium hydroxide alkali glue catalyst is decomposed in the heating of kettle 1, and the material after reaction is evacuated to horizontal rotary by conveyance conduit and is steamed
It sends out in device 2, the n-hexane of 50 parts by weight is knocked down in horizontal rotary evaporator 2 by the 4th material inlet 2-2, open vacuum
To -0.06MPa hereinafter, gradually to azeotropic temperature up to 180 DEG C of progress azeotropic reactions, abjection low molecule obtains silicone oil for temperature-gradient method
Finished product E, the steam that azeotropic generates enter condenser 3 by jet chimney, the azeotropic solvent and D3-D20 of different boiling after condensation
Small-molecule substance respectively enters the second sub- recycling can 4 and the first sub- recycling can 5 through triple valve 7, and the first sub- recycling can is for recycling
Azeotropic solvent, the second sub- recycling can is for recycling D3-D20 small-molecule substance.
Embodiment 2
The embodiment of the present invention provides second of synthetic method of high purity silicone oil, specifically:
As shown in Figure 1, the embodiment of the invention provides the synthesizers of high purity silicone oil, comprising: reaction kettle 1, horizontal rotation
Turn evaporator 2, condenser 3, triple valve 7, the second sub- recycling can 4, the first sub- recycling can 5；Reaction kettle exports 1-1 and horizontal rotary
Evaporator 2-1 is connected by pipeline, and the bottom of horizontal rotary evaporator 2 is equipped with high purity silicon oil export 2-4, horizontal rotary
The top of evaporator 2 is equipped with the 4th material inlet 2-2；Horizontal rotary evaporator outlet 2-3 and condenser inlet 3-1 pass through pipeline
Connection；Condensator outlet 3-2 is connect with the second sub- recycling can 4 and the first sub- 5 pipeline of recycling can respectively by triple valve 7.
In the synthesizer of the high purity silicone oil of the embodiment of the present invention, by the octamethylcy-clotetrasiloxane of 100 parts by weight
It is knocked down in reaction kettle 1 by the first material inlet A, is warming up to 60 DEG C, open vacuum to -0.06MPa hereinafter, dehydration 30 minutes,
The tetramethylammonium hydroxide alkali glue of the hexamethyldisiloxane closure agent of 5 parts by weight and 0.02 parts by weight is passed through into the second original respectively
Material import B and third material inlet C is knocked down in reaction kettle 1, is warming up to balanced reaction 4 hours at 105-115 DEG C, and 1 liter of reaction kettle
Temperature decomposes tetramethylammonium hydroxide alkali glue catalyst, and the material after reaction is evacuated to horizontal rotary evaporator 2 by conveyance conduit
In, the pentane of 80 parts by weight is knocked down in horizontal rotary evaporator 2 by the 4th material inlet 2-2, open vacuum to-
0.06MPa hereinafter, gradually temperature-gradient method deviate from low molecule to the temperature of azeotropic up to 180 DEG C of progress azeotropic reactions, obtain silicone oil at
Product E, the steam that azeotropic generates enter condenser 3 by jet chimney, and the azeotropic solvent and D3-D20 of different boiling are small after condensation
Molecular substance respectively enters the second sub- recycling can 4 and the first sub- recycling can 5 through triple valve 7, and the first sub- recycling can is for recycling altogether
Boil-off dose, the second sub- recycling can is for recycling D3-D20 small-molecule substance.
Embodiment 3
The embodiment of the present invention provides the third synthetic method of high purity silicone oil, specifically:
As shown in Figure 1, the embodiment of the invention provides the synthesizers of high purity silicone oil, comprising: reaction kettle 1, horizontal rotation
Turn evaporator 2, condenser 3, triple valve 7, the second sub- recycling can 4, the first sub- recycling can 5；Reaction kettle exports 1-1 and horizontal rotary
Evaporator 2-1 is connected by pipeline, and the bottom of horizontal rotary evaporator 2 is equipped with high purity silicon oil export 2-4, horizontal rotary
The top of evaporator 2 is equipped with the 4th material inlet 2-2；Horizontal rotary evaporator outlet 2-3 and condenser inlet 3-1 pass through pipeline
Connection；Condensator outlet 3-2 is connect with the second sub- recycling can 4 and the first sub- 5 pipeline of recycling can respectively by triple valve 7.
In the synthesizer of the high purity silicone oil of the embodiment of the present invention, by the methyl hydrogen siloxane ring body of 100 parts by weight
(D4H) it is knocked down in reaction kettle 1 by the first material inlet A, by the hexamethyldisiloxane closure agent and 5 parts by weight of 5 parts by weight
Resin cation pass through the second material inlet B respectively and third material inlet C is knocked down in reaction kettle 1, be warming up at 80 DEG C and put down
Weighing apparatus reaction 4 hours, after the material filtering after reaction, is evacuated to horizontal rotary evaporator by conveyance conduit for filtered material
In 2, the pentane of 50 parts by weight is knocked down in horizontal rotary evaporator 2 by the 4th material inlet 2-2, open vacuum to-
For 0.06MPa hereinafter, gradually temperature-gradient method to the temperature of azeotropic carries out azeotropic reaction up to 150 DEG C, abjection low molecule obtains silicone oil
Finished product E, the steam that azeotropic generates enter condenser 3 by jet chimney, the azeotropic solvent and D3-D20 of different boiling after condensation
Small-molecule substance respectively enters the second sub- recycling can 4 and the first sub- recycling can 5 through triple valve 7, and the first sub- recycling can is for recycling
Azeotropic solvent, the second sub- recycling can is for recycling D3-D20 small-molecule substance.
Embodiment 4
The present embodiment is that the silicone oil finished product obtained to embodiment 1-3 carries out viscosity, fugitive constituent and D3-D20 small molecule ring
The detection of body content, the specific steps are as follows:
Silicone oil finished product in embodiment 1-3 is volatilized according to existing conventional method through gas chromatography and 200 DEG C/4 hours
Test, during result is tabulated below:
| Test item | Conventional silicone oil | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Viscosity (mPa.s) | 500 | 500 | 300 | 80 |
| Fugitive constituent | 1.8% | 0.2% | 0.13% | 0.22% |
| D3-D20 small molecule ring body content | 1.2% | < 0.1% | < 0.1% | < 0.1% |
Note: the preparation method of conventional silicone oil, similar with the preparation method of silicone oil finished product in embodiment 1, difference is to be not added
The octamethylcy-clotetrasiloxane of 100 parts by weight is knocked down in reaction kettle 1 by the first material inlet A, is warming up to 60 by azeotropic solvent
DEG C, open vacuum under -0.06MPa, be dehydrated 30 minutes, by the tetramethyl divinyl siloxanes closure agent of 2 parts by weight and
The tetramethylammonium hydroxide alkali glue of 0.02 parts by weight passes through the second material inlet B respectively and third material inlet C knocks down reaction kettle 1
In, balanced reaction 4 hours at 180-200 DEG C are warming up to, tetramethylammonium hydroxide alkali glue catalyst, In are decomposed in the heating of reaction kettle 1
Synthetic reaction is completed to obtain product 1, and product 1 directly in a kettle, opens vacuum to -0.06MPa hereinafter, being warming up to 180-
200 DEG C of abjection small-molecule substances obtain conventional silicone oil.
As can be known from the above table, fugitive constituent can be synthesized using synthetic method of the invention and D3-D20 small molecule ring body content is low
High purity silicone oil.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of synthetic method of high purity silicone oil, which comprises the following steps:
Polysiloxanes ring body, end-capping reagent and catalyst are mixed and are reacted by step 1, obtain reactant 1；
Step 2 after removing the catalyst of the reactant 1, obtains product 1；
Step 3 mixes the product 1 with azeotropic solvent, carries out azeotropic processing, obtains high purity silicone oil.
2. the synthetic method of high purity silicone oil according to claim 1, which is characterized in that the polysiloxanes ring body is selected from
Dimethicone, methylvinylcyclosiloxane, methyl phenyl ring siloxane, hexichol cyclosiloxane, methyl trifluoro third
One of cyclosiloxane and methylhydracyclosiloxane are a variety of.
3. the synthetic method of high purity silicone oil according to claim 1, which is characterized in that the end-capping reagent is selected from hexamethyl
One of disiloxane, methyl ethylene disiloxane and methyl hydrogen disiloxane are a variety of.
4. the synthetic method of high purity silicone oil according to claim 1, which is characterized in that the catalyst is urged selected from acidity
One of agent, basic catalyst or solid catalyst.
5. the synthetic method of high purity silicone oil according to claim 1, which is characterized in that the azeotropic solvent is that boiling point exists
200 DEG C of organic alkanes below.
6. the synthetic method of high purity silicone oil according to claim 5, which is characterized in that the azeotropic solvent is selected from penta
One of alkane, hexane, heptane, octane and nonane are a variety of.
7. the synthetic method of high purity silicone oil according to claim 1, which is characterized in that the azeotropic solvent and the production
The weight ratio of object 1 is (5-200): 100.
8. the synthetic method of high purity silicone oil according to claim 1, which is characterized in that include: in step 1
Step 1a, decompression dehydration processing will be carried out after the heating of polysiloxanes ring body, obtains product one；
Step 1b, the product one is reacted with end-capping reagent and catalyst Hybrid Heating, obtains reactant 1.
9. a kind of synthesizer of the high purity silicone oil as described in claim 1-8 any one characterized by comprising
Reaction kettle, horizontal rotary evaporator, condenser and recycling can；
The reaction kettle is connect with the horizontal rotary evaporator pipeline, and the bottom of the horizontal-type evaporator is exported equipped with silicone oil,
The top of the horizontal rotary evaporator is equipped with material inlet；
The horizontal rotary evaporator is connect with the condenser tubes；
The condenser is connect with the recycling can pipeline.
10. synthesizer according to claim 9, which is characterized in that the horizontal rotary evaporator is long greater than high
Rotary evaporator.
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Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB788151A (en) * | 1953-10-19 | 1957-12-23 | Du Pont | Solid siliceous materials of high surface area, methods of making the same, and compositions containing them |
| JPH09150002A (en) * | 1995-11-29 | 1997-06-10 | Shin Etsu Chem Co Ltd | Purification method of silicone oil |
| US20030212286A1 (en) * | 2002-05-13 | 2003-11-13 | Hiroshi Nakayama | Purification of silicone oil |
| CN201791386U (en) * | 2010-09-08 | 2011-04-13 | 郑州拓洋生物工程有限公司 | Horizontal evaporator |
| CN102079816A (en) * | 2009-11-27 | 2011-06-01 | 威海赛奥新材料科技有限公司 | Preparation method of high purity silicone oil |
| CN102898646A (en) * | 2012-09-06 | 2013-01-30 | 江苏梅兰化工有限公司 | Continuous production process for silicone oil |
| CN107778488A (en) * | 2017-11-16 | 2018-03-09 | 湖北兴瑞化工有限公司 | A kind of de- low molecule device and the method that production viscosity is 30 1000000cs methyl-silicone oils |
| CN108102100A (en) * | 2017-12-27 | 2018-06-01 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low volatilization vinyl silicone oil |
| CN108484913A (en) * | 2018-03-07 | 2018-09-04 | 江苏科幸新材料股份有限公司 | The preparation method of high-purity ethylene base silicone oil |
| CN108610484A (en) * | 2018-05-25 | 2018-10-02 | 广州盛泰诺新材料科技有限公司 | A kind of thermostable transparent methyl-silicone oil and its synthetic method |
| CN108610483A (en) * | 2018-05-25 | 2018-10-02 | 广州盛泰诺新材料科技有限公司 | A kind of high-purity dimethicone of resistance to oxidation and its synthetic method |
-
2019
- 2019-08-27 CN CN201910797498.1A patent/CN110483776B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB788151A (en) * | 1953-10-19 | 1957-12-23 | Du Pont | Solid siliceous materials of high surface area, methods of making the same, and compositions containing them |
| JPH09150002A (en) * | 1995-11-29 | 1997-06-10 | Shin Etsu Chem Co Ltd | Purification method of silicone oil |
| US20030212286A1 (en) * | 2002-05-13 | 2003-11-13 | Hiroshi Nakayama | Purification of silicone oil |
| CN102079816A (en) * | 2009-11-27 | 2011-06-01 | 威海赛奥新材料科技有限公司 | Preparation method of high purity silicone oil |
| CN201791386U (en) * | 2010-09-08 | 2011-04-13 | 郑州拓洋生物工程有限公司 | Horizontal evaporator |
| CN102898646A (en) * | 2012-09-06 | 2013-01-30 | 江苏梅兰化工有限公司 | Continuous production process for silicone oil |
| CN107778488A (en) * | 2017-11-16 | 2018-03-09 | 湖北兴瑞化工有限公司 | A kind of de- low molecule device and the method that production viscosity is 30 1000000cs methyl-silicone oils |
| CN108102100A (en) * | 2017-12-27 | 2018-06-01 | 浙江福斯特新材料研究院有限公司 | A kind of production method and production system of low volatilization vinyl silicone oil |
| CN108484913A (en) * | 2018-03-07 | 2018-09-04 | 江苏科幸新材料股份有限公司 | The preparation method of high-purity ethylene base silicone oil |
| CN108610484A (en) * | 2018-05-25 | 2018-10-02 | 广州盛泰诺新材料科技有限公司 | A kind of thermostable transparent methyl-silicone oil and its synthetic method |
| CN108610483A (en) * | 2018-05-25 | 2018-10-02 | 广州盛泰诺新材料科技有限公司 | A kind of high-purity dimethicone of resistance to oxidation and its synthetic method |
Non-Patent Citations (2)
| Title |
|---|
| 刘士星等: "《化工原理》", 31 August 1994, 中国科学技术大学出版社 * |
| 应卫勇等: "《碳一化工主要产品生产技术》", 31 March 2004, 化学工业出版社 * |
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