CN108383865A - The system and method for vapor- phase synthesis Ethoxysilane - Google Patents
The system and method for vapor- phase synthesis Ethoxysilane Download PDFInfo
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- CN108383865A CN108383865A CN201810182251.4A CN201810182251A CN108383865A CN 108383865 A CN108383865 A CN 108383865A CN 201810182251 A CN201810182251 A CN 201810182251A CN 108383865 A CN108383865 A CN 108383865A
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- tubular reactor
- pipeline
- feed
- receiver
- ethoxysilane
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- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 23
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 23
- CWAFVXWRGIEBPL-UHFFFAOYSA-N ethoxysilane Chemical compound CCO[SiH3] CWAFVXWRGIEBPL-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000012808 vapor phase Substances 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 21
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000003054 catalyst Substances 0.000 claims abstract description 24
- 235000019441 ethanol Nutrition 0.000 claims abstract description 21
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 12
- 238000011049 filling Methods 0.000 claims abstract description 9
- 239000012263 liquid product Substances 0.000 claims abstract description 6
- 239000002808 molecular sieve Substances 0.000 claims description 25
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 17
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 15
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 11
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 239000007864 aqueous solution Substances 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- -1 siloxanes Chemical class 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- VVTSZOCINPYFDP-UHFFFAOYSA-N [O].[Ar] Chemical compound [O].[Ar] VVTSZOCINPYFDP-UHFFFAOYSA-N 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 description 9
- 238000002329 infrared spectrum Methods 0.000 description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 3
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 3
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- KSCAZPYHLGGNPZ-UHFFFAOYSA-N 3-chloropropyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)CCCCl KSCAZPYHLGGNPZ-UHFFFAOYSA-N 0.000 description 1
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- ZZHNUBIHHLQNHX-UHFFFAOYSA-N butoxysilane Chemical compound CCCCO[SiH3] ZZHNUBIHHLQNHX-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 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
- C07F7/025—Silicon compounds without C-silicon linkages
-
- 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
- C07F7/04—Esters of silicic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses the systems of vapor- phase synthesis Ethoxysilane, including the first container, second container, the first metering pump, the second metering pump, tubular reactor, electric heater, PID temperature controller, cooling tube, receiver, buffer and exhaust scrubber.The invention also discloses the methods of vapor- phase synthesis Ethoxysilane, including (1) prepares catalyst；(2) catalyst is placed in the filling section of tubular reactor；(3) it is passed through ethyl alcohol and disilicone hexachloride simultaneously to tubular reactor, controls the reaction temperature of tubular reactor at 250~450 DEG C, wherein：The molar ratio of ethyl alcohol and disilicone hexachloride=(7~20):1；Mass space velocity is controlled in 1~20h‑1；(4) reaction product enters receiver after cooling tube cools down, and in the receiver, gas tail gas discharges liquid product collection after being washed by exhaust scrubber after buffer.The reaction of the present invention carries out under atmospheric low-temperature, safety coefficient higher.
Description
Technical field
The invention belongs to Materials Science and Engineering fields, and in particular to the system and method for vapor- phase synthesis Ethoxysilane.
Background technology
After hydrogen atom in silane in Si -- H bond is replaced by alkoxy, referred to as alkoxy silane, such as methoxy silane, ethoxy
Base silane, npropoxysilane, butoxy silane etc..According to different degree of substitution, and an alkoxy silane, dialkoxy can be divided into
Silane, trialkoxy silane and tetraalkoxysilane.
Alkoxy silane is important organosilicon materials, and wherein triethoxysilane can synthesize such as three ethoxy of aminopropyl
A series of silane such as base silane, chloropropyl triethoxysilane, vinyltriethoxysilane, mercaptopropyltriethoxysilane are even
Join agent, is raw material midbody important in coupling agent preparation process.Tetraethoxysilane and its condensation polymer are in resin, coating, oil
The occasions such as paint, catalyst have important application.
The traditional synthetic method of triethoxysilane is to carry out liquid phase alcoholysis reaction system as raw material using trichlorosilane and ethyl alcohol
It is standby to obtain；The prior synthesizing method of tetraethoxysilane and its condensation polymer is to carry out liquid phase reactor preparation with silicon tetrachloride and ethyl alcohol
It obtains.But the above method has the following disadvantages：It is led using the gap reaction of tank reactor or semicontinuous reactive mode
Cause production efficiency lower；The gas phase and liquid phase mixture that hydrogen chloride and ethyl alcohol are formed in liquid-phase reaction system are in dew-point temperature
Hereinafter, cause hydrogen chloride that can form strong corrosivity, therefore reactor must use glass-lined equipment, and glass-lined equipment
Using again cause the production scale of single production line to be restricted.
Scientific research personnel develops the direct method technique using metallic silicon power as raw material in recent years, and this method is under high temperature, high pressure
The liquid-solid reaction Direct Synthesis of Triethoxyl Silane or tetraethoxysilane of silica flour and alcohol are realized by the effect of Cu-series catalyst.
But the above method has the following disadvantages：Reaction carries out under suitable high pressure, and reaction process danger is larger.
Invention content
Goal of the invention：The present invention has made improvements in view of the above-mentioned problems of the prior art, i.e. the first object of the present invention
It is the system of open vapor- phase synthesis Ethoxysilane.Second object of the present invention is open vapor- phase synthesis Ethoxysilane
Method.
Technical solution：The system of vapor- phase synthesis Ethoxysilane, including：
The first container, for storing disilicone hexachloride；
Second container, for storing ethyl alcohol；
First metering pump, feed inlet are connected with the first container by pipeline；
Second metering pump, feed inlet are connected with second container by pipeline；
Tubular reactor, feed end are set there are two feed-inputing branched pipe, two feed-inputing branched pipes respectively with the first metering pump
Discharge port, the second metering pump discharge port be connected by pipeline, the middle part of tubular reactor, which is equipped with, loads section, in loading section
Equipped with catalyst；
Electric heater is wrapped in the feed-inputing branched pipe of tubular reactor, loads the outside of section；
PID temperature controller, is connected with electric heater, the heating temperature for controlling electric heater；
Cooling tube, one end are connected with the discharge end of tubular reactor by pipeline；
Receiver, feed end are connected with the other end of cooling tube by pipeline；
Buffer, feed end are connected with the discharge end of receiver by pipeline；
Exhaust scrubber, feed end are connected with the discharge end of buffer by pipeline, the discharge end of exhaust scrubber
It is communicated by pipeline with the external world.
The method of vapor- phase synthesis Ethoxysilane, includes the following steps：
(1) catalyst is prepared
(11) 1~3 mass parts copper nitrate is dissolved in 3 mass parts deionized waters and forms copper nitrate aqueous solution；
(12) 0.5~2 mass parts Si-MCM-41 molecular sieves are placed in the copper nitrate aqueous solution that step (1) obtains, 20
At~300 DEG C dipping 1~for 24 hours, subsequently into step (13)；
(13) the Si-MCM-41 molecular sieves after solid-liquor separation and drying impregnate, subsequently into step (14)；
(14) in a hydrogen atmosphere by the Si-MCM-41 molecular sieves after drying, it is heat-treated 1~5h at 650 DEG C, is loaded
The Si-MCM-41 molecular sieves of copper, subsequently into step (15)；
(15) by the Si-MCM-41 molecular sieves of supported copper at 150~300 DEG C, the oxygen-of oxygen content 1~5% (v/v)
1~5h is heat-treated in the mixed atmosphere of argon gas to get to catalyst；
(2) catalyst prepared by step (1) is placed in the filling section of tubular reactor, subsequently into step (3)；
(3) it is passed through ethyl alcohol and disilicone hexachloride simultaneously to tubular reactor, controls the reaction temperature of tubular reactor 250
~450 DEG C, wherein：
The molar ratio of ethyl alcohol and disilicone hexachloride=(7~20):1；
Mass space velocity is controlled in 1~20h-1；
(4) reaction product after cooling tube cools down enter receiver, liquid product collection in the receiver, gas tail gas
It is discharged after being washed by exhaust scrubber after buffer.
Further, step (4) obtained reaction product includes triethoxysilane, tetraethoxysilane and six second
Oxygroup second siloxanes.
Advantageous effect：The system and method for vapor- phase synthesis Ethoxysilane disclosed by the invention has the advantages that：
1, using gas phase successive reaction mode, the more existing liquid phase gap reactive mode of reaction efficiency is high；Due to reacting
Cheng Wendu is more than the dew-point temperature of ethanolic hydrogen chloride system, therefore equipment material can use metal material；Exactly because also may be used
To use metal material, therefore the optional range of reactor size is wider compared with enamel still reactor, what single production line scale can be done
Bigger.
2, reaction process is carried out in normal pressure, and the reaction under high pressure relative to direct method is safer.
Description of the drawings
Fig. 1 is the structural schematic diagram of the system of vapor- phase synthesis Ethoxysilane disclosed by the invention；
Fig. 2 a are the product of an embodiment of the method for vapor- phase synthesis Ethoxysilane disclosed by the invention at 133-135 DEG C
Fraction infrared spectrum；
Fig. 2 b are the infrared spectrum of triethoxysilane；
Fig. 2 c are the product of an embodiment of the method for vapor- phase synthesis Ethoxysilane disclosed by the invention at 165-168 DEG C
Fraction infrared spectrum；
Fig. 2 d are the infrared spectrum of tetraethoxysilane.
Wherein：
1- the first container 2- second containers
3- the first metering pump the second metering pumps of 4-
5- electric heater 6- tubular reactors
7- loads section 8- cooling tubes
9- receiver 10-PID temperature controllers
11- buffer 12- exhaust scrubbers
Specific implementation mode：
The specific implementation mode of the present invention is described in detail below.
Specific embodiment 1
As shown in Figure 1, the system of vapor- phase synthesis Ethoxysilane, including：
The first container 1, for storing disilicone hexachloride；
Second container 2, for storing ethyl alcohol；
First metering pump 3, feed inlet are connected with the first container 1 by pipeline；
Second metering pump 4, feed inlet are connected with second container 2 by pipeline；
Tubular reactor 6, feed end are set there are two feed-inputing branched pipe, two feed-inputing branched pipes respectively with the first metering pump 3
Discharge port, the second metering pump 4 discharge port be connected by pipeline, the middle part of tubular reactor 6, which is equipped with, loads section 7, is filling out
It fills and catalyst is housed in section 7；
Electric heater 5 is wrapped in the feed-inputing branched pipe of tubular reactor 6, loads the outside of section 7；
PID temperature controller 10 is connected with electric heater 5, the heating temperature for controlling electric heater 5；
Cooling tube 8, one end are connected with the discharge end of tubular reactor 6 by pipeline；
Receiver 9, feed end are connected with the other end of cooling tube 8 by pipeline；
Buffer 11, feed end are connected with the discharge end of receiver 9 by pipeline；
Exhaust scrubber 12, feed end are connected with the discharge end of buffer 11 by pipeline, exhaust scrubber 12
Discharge end is communicated with the external world by pipeline.
The method of vapor- phase synthesis Ethoxysilane, includes the following steps：
(1) catalyst is prepared
(11) 2 mass parts copper nitrates are dissolved in 3 mass parts deionized waters and form copper nitrate aqueous solution；
(12) 1 mass parts Si-MCM-41 molecular sieves are placed in the copper nitrate aqueous solution that step (1) obtains, at 160 DEG C
12h is impregnated, subsequently into step (13)；
(13) the Si-MCM-41 molecular sieves after solid-liquor separation and drying impregnate, subsequently into step (14)；
(14) in a hydrogen atmosphere by the Si-MCM-41 molecular sieves after drying, it is heat-treated 3h at 650 DEG C, obtains supported copper
Si-MCM-41 molecular sieves, subsequently into step (15)；
(15) by the Si-MCM-41 molecular sieves of supported copper at 230 DEG C, oxygen-argon gas of oxygen content 3% (v/v) mixes
Heat treatment 3h is closed in atmosphere to get to catalyst；
(2) catalyst prepared by step (1) is placed in the filling section of tubular reactor, subsequently into step (3)；
(3) it is passed through ethyl alcohol and disilicone hexachloride simultaneously to tubular reactor, controls the reaction temperature of tubular reactor 350
DEG C, wherein：
Molar ratio=15 of ethyl alcohol and disilicone hexachloride:1；
Mass space velocity is controlled in 10h-1；
(4) reaction product after cooling tube cools down enter receiver, liquid product collection in the receiver, gas tail gas
It is discharged after being washed by exhaust scrubber after buffer.
Further, step (4) obtained reaction product includes triethoxysilane, tetraethoxysilane and six second
Oxygroup second siloxanes.
Into the reaction product obtained by step (4) through atmospheric distillation, 133~135 DEG C and 165~168 DEG C of fraction is intercepted,
The fraction is through infrared analysis, and infared spectrum is as shown in Fig. 2 a, Fig. 2 c.By the comparison of infrared spectrum (triethoxysilane and
The infrared spectrum of tetraethoxysilane is as shown in Fig. 2 b and 2d), it can be determined that 133~135 DEG C of fraction is triethoxysilane,
And 165~168 DEG C of fraction is tetraethoxysilane.
Specific embodiment 2
As shown in Figure 1, the system of vapor- phase synthesis Ethoxysilane, including：
The first container 1, for storing disilicone hexachloride；
Second container 2, for storing ethyl alcohol；
First metering pump 3, feed inlet are connected with the first container 1 by pipeline；
Second metering pump 4, feed inlet are connected with second container 2 by pipeline；
Tubular reactor 6, feed end are set there are two feed-inputing branched pipe, two feed-inputing branched pipes respectively with the first metering pump 3
Discharge port, the second metering pump 4 discharge port be connected by pipeline, the middle part of tubular reactor 6, which is equipped with, loads section 7, is filling out
It fills and catalyst is housed in section 7；
Electric heater 5 is wrapped in the feed-inputing branched pipe of tubular reactor 6, loads the outside of section 7；
PID temperature controller 10 is connected with electric heater 5, the heating temperature for controlling electric heater 5；
Cooling tube 8, one end are connected with the discharge end of tubular reactor 6 by pipeline；
Receiver 9, feed end are connected with the other end of cooling tube 8 by pipeline；
Buffer 11, feed end are connected with the discharge end of receiver 9 by pipeline；
Exhaust scrubber 12, feed end are connected with the discharge end of buffer 11 by pipeline, exhaust scrubber 12
Discharge end is communicated with the external world by pipeline.
The method of vapor- phase synthesis Ethoxysilane, includes the following steps：
(1) catalyst is prepared
(11) 1 mass parts copper nitrate is dissolved in 3 mass parts deionized waters and forms copper nitrate aqueous solution；
(12) 0.5 mass parts Si-MCM-41 molecular sieves are placed in the copper nitrate aqueous solution that step (1) obtains, at 20 DEG C
It is lower to impregnate for 24 hours, subsequently into step (13)；
(13) the Si-MCM-41 molecular sieves after solid-liquor separation and drying impregnate, subsequently into step (14)；
(14) in a hydrogen atmosphere by the Si-MCM-41 molecular sieves after drying, it is heat-treated 1h at 650 DEG C, obtains supported copper
Si-MCM-41 molecular sieves, subsequently into step (15)；
(15) by the Si-MCM-41 molecular sieves of supported copper at 150 DEG C, oxygen-argon gas of oxygen content 5% (v/v) mixes
Heat treatment 1h is closed in atmosphere to get to catalyst；
(2) catalyst prepared by step (1) is placed in the filling section of tubular reactor, subsequently into step (3)；
(3) it is passed through ethyl alcohol and disilicone hexachloride simultaneously to tubular reactor, controls the reaction temperature of tubular reactor 250
DEG C, wherein：
Molar ratio=7 of ethyl alcohol and disilicone hexachloride:1；
Mass space velocity is controlled in 1h-1；
(4) reaction product after cooling tube cools down enter receiver, liquid product collection in the receiver, gas tail gas
It is discharged after being washed by exhaust scrubber after buffer.
Further, step (4) obtained reaction product includes triethoxysilane, tetraethoxysilane and six second
Oxygroup second siloxanes.
Specific embodiment 3
As shown in Figure 1, the system of vapor- phase synthesis Ethoxysilane, including：
The first container 1, for storing disilicone hexachloride；
Second container 2, for storing ethyl alcohol；
First metering pump 3, feed inlet are connected with the first container 1 by pipeline；
Second metering pump 4, feed inlet are connected with second container 2 by pipeline；
Tubular reactor 6, feed end are set there are two feed-inputing branched pipe, two feed-inputing branched pipes respectively with the first metering pump 3
Discharge port, the second metering pump 4 discharge port be connected by pipeline, the middle part of tubular reactor 6, which is equipped with, loads section 7, is filling out
It fills and catalyst is housed in section 7；
Electric heater 5 is wrapped in the feed-inputing branched pipe of tubular reactor 6, loads the outside of section 7；
PID temperature controller 10 is connected with electric heater 5, the heating temperature for controlling electric heater 5；
Cooling tube 8, one end are connected with the discharge end of tubular reactor 6 by pipeline；
Receiver 9, feed end are connected with the other end of cooling tube 8 by pipeline；
Buffer 11, feed end are connected with the discharge end of receiver 9 by pipeline；
Exhaust scrubber 12, feed end are connected with the discharge end of buffer 11 by pipeline, exhaust scrubber 12
Discharge end is communicated with the external world by pipeline.
The method of vapor- phase synthesis Ethoxysilane, includes the following steps：
(1) catalyst is prepared
(11) 3 mass parts copper nitrates are dissolved in 3 mass parts deionized waters and form copper nitrate aqueous solution；
(12) 2 mass parts Si-MCM-41 molecular sieves are placed in the copper nitrate aqueous solution that step (1) obtains, at 300 DEG C
1h is impregnated, subsequently into step (13)；
(13) the Si-MCM-41 molecular sieves after solid-liquor separation and drying impregnate, subsequently into step (14)；
(14) in a hydrogen atmosphere by the Si-MCM-41 molecular sieves after drying, it is heat-treated 5h at 650 DEG C, obtains supported copper
Si-MCM-41 molecular sieves, subsequently into step (15)；
(15) by the Si-MCM-41 molecular sieves of supported copper at 300 DEG C, oxygen-argon gas of oxygen content 1% (v/v) mixes
Heat treatment 1h is closed in atmosphere to get to catalyst；
(2) catalyst prepared by step (1) is placed in the filling section of tubular reactor, subsequently into step (3)；
(3) it is passed through ethyl alcohol and disilicone hexachloride simultaneously to tubular reactor, controls the reaction temperature of tubular reactor 450
DEG C, wherein：
Molar ratio=20 of ethyl alcohol and disilicone hexachloride:1；
Mass space velocity is controlled in 20h-1；
(4) reaction product after cooling tube cools down enter receiver, liquid product collection in the receiver, gas tail gas
It is discharged after being washed by exhaust scrubber after buffer.
Further, step (4) obtained reaction product includes triethoxysilane, tetraethoxysilane and six second
Oxygroup second siloxanes.
Embodiments of the present invention are elaborated above.But present invention is not limited to the embodiments described above,
Technical field those of ordinary skill within the scope of knowledge, can also do without departing from the purpose of the present invention
Go out various change.
Claims (3)
1. the system of vapor- phase synthesis Ethoxysilane, which is characterized in that including：
The first container, for storing disilicone hexachloride；
Second container, for storing ethyl alcohol；
First metering pump, feed inlet are connected with the first container by pipeline；
Second metering pump, feed inlet are connected with second container by pipeline；
Tubular reactor, feed end are set there are two feed-inputing branched pipe, two feed-inputing branched pipes discharging with the first metering pump respectively
Mouthful, the discharge port of the second metering pump be connected by pipeline, the middle part of tubular reactor, which is equipped with, loads section, is equipped in loading section
Catalyst；
Electric heater is wrapped in the feed-inputing branched pipe of tubular reactor, loads the outside of section；
PID temperature controller, is connected with electric heater, the heating temperature for controlling electric heater；
Cooling tube, one end are connected with the discharge end of tubular reactor by pipeline；
Receiver, feed end are connected with the other end of cooling tube by pipeline；
Buffer, feed end are connected with the discharge end of receiver by pipeline；
Exhaust scrubber, feed end are connected with the discharge end of buffer by pipeline, the discharge end of exhaust scrubber with it is outer
Boundary is communicated by pipeline.
2. the method for vapor- phase synthesis Ethoxysilane, which is characterized in that include the following steps：
(1) catalyst is prepared
(11) 1~3 mass parts copper nitrate is dissolved in 3 mass parts deionized waters and forms copper nitrate aqueous solution；
(12) 0.5~2 mass parts Si-MCM-41 molecular sieves are placed in the copper nitrate aqueous solution that step (1) obtains, 20~
At 300 DEG C dipping 1~for 24 hours, subsequently into step (13)；
(13) the Si-MCM-41 molecular sieves after solid-liquor separation and drying impregnate, subsequently into step (14)；
(14) in a hydrogen atmosphere by the Si-MCM-41 molecular sieves after drying, it is heat-treated 1~5h at 650 DEG C, obtains supported copper
Si-MCM-41 molecular sieves, subsequently into step (15)；
(15) by the Si-MCM-41 molecular sieves of supported copper at 150~300 DEG C, oxygen-argon gas of oxygen content 1~5% (v/v)
Mixed atmosphere in 1~5h of heat treatment to get to catalyst；
(2) catalyst prepared by step (1) is placed in the filling section of tubular reactor, subsequently into step (3)；
(3) ethyl alcohol and disilicone hexachloride are passed through simultaneously to tubular reactor, control the reaction temperature of tubular reactor 250~
450 DEG C, wherein：
The molar ratio of ethyl alcohol and disilicone hexachloride=(7~20):1；
Mass space velocity is controlled in 1~20h-1；
(4) reaction product enters receiver after cooling tube cools down, and in the receiver, gas tail gas passes through liquid product collection
It is discharged after being washed by exhaust scrubber after buffer.
3. the method for vapor- phase synthesis Ethoxysilane according to claim 2, which is characterized in that step (4) is obtained
Reaction product includes triethoxysilane, tetraethoxysilane and six ethyoxyl second siloxanes.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112280038A (en) * | 2020-10-28 | 2021-01-29 | 廉江市政业新材料有限公司 | Method for converting impurities in alkoxy silane product |
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