CN104437295B - Prepare the device and method of tetramethoxy-silicane - Google Patents
Prepare the device and method of tetramethoxy-silicane Download PDFInfo
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- CN104437295B CN104437295B CN201410816621.7A CN201410816621A CN104437295B CN 104437295 B CN104437295 B CN 104437295B CN 201410816621 A CN201410816621 A CN 201410816621A CN 104437295 B CN104437295 B CN 104437295B
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- tetramethoxy
- silicane
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- reactive distillation
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- 238000000034 method Methods 0.000 title claims abstract description 33
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 115
- 239000007788 liquid Substances 0.000 claims abstract description 77
- 238000006243 chemical reaction Methods 0.000 claims abstract description 45
- 238000000066 reactive distillation Methods 0.000 claims abstract description 39
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000011027 product recovery Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 35
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 35
- 238000009835 boiling Methods 0.000 claims description 21
- 239000000945 filler Substances 0.000 claims description 18
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000000919 ceramic Substances 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 22
- 238000000605 extraction Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 239000006227 byproduct Substances 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- 239000000376 reactant Substances 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 229910000077 silane Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000004044 response Effects 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000012043 crude product Substances 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 230000002459 sustained effect Effects 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- -1 tetramethyl TMOS Chemical compound 0.000 description 2
- 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
- 241000208340 Araliaceae Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005304 optical glass Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
- B01J8/025—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical in a cylindrical shaped bed
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Fluid Mechanics (AREA)
- Silicon Compounds (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides the device and method preparing tetramethoxy-silicane, relate to tetramethoxy-silicane preparation field.This device includes reactive distillation column, reboiler and overhead condenser；It is respectively rectifying section, conversion zone and stripping section in reactive distillation column from top to bottom, the outer wall residing for conversion zone is provided with methanol inlet port and Silicon chloride. inlet port；The bottom of reactive distillation column is provided with on tower bottom outlet, and tower bottom outlet and is provided with liquid output pipe；Outside reboiler is arranged at the bottom of the tower of reactive distillation column, its one end connects with tower bottom outlet pipe, and the other end connects with stripping section；Overhead condenser is arranged on the top of reactive distillation column, and its one end connects with the top exit of reactive distillation column, and the other end connects overhead product recovery tube and a liquid return tube connected with rectifying section.Reaction and two kinds of equipment of separation are united two into one by this device, and the technique simplifying complexity reduces equipment investment and operating cost.
Description
Technical field
The present invention relates to tetramethoxy-silicane preparation field, prepare in particular to one
The device and method of tetramethoxy-silicane.
Background technology
Tetramethoxy-silicane can synthesize as organosilicon, heat resistant paint manufacture, binding agent, electronics
The insulant in the fields such as industry, is also the important former of optical glass inorganic agent and coagulating agent etc.
Material；It is widely used, so its synthesis is constantly subjected to the concern of chemical industry.
Traditional synthetic method is by Silicon chloride. and the direct liquid phase reactor of methanol, by controlling four
Silicon chloride and the burden control response speed of methanol, the tetramethoxy-silicane of generation needs to pass through
Further rectification and purification technique can reach the purity of more than 99%.This kind of traditional tetramethyl
TMOS synthetic method its be divided into two operating processes, be first the stage of being synthesized, its
The secondary stage being to carry out the crude product of synthesis purifying (i.e. separating).Raw at concrete chemical industry
In product, it is synthesized with separating-purifying two kinds operation generally respectively in the two single equipment of class
Carry out；I.e. synthesize crude product first with consersion unit, the most again crude product is input to another
Equipment for purifying carries out purification processes.
Therefore, traditional prepares tetramethoxy-silicane equipment, due to synthesis and separating-purifying
Equipment is to be separately provided, and therefore there is whole preparation technology and operates complexity, long flow path, equipment
The problems such as investment is big, yield is low, energy consumption is high, and then also result in tetramethoxy-silicane synthesis
Inefficiency, price is up to more than 10,000 yuan per ton, limits application, and cause downstream
Product cost rises.
In view of this, the special proposition present invention.
Summary of the invention
The first object of the present invention is to provide a kind of device preparing tetramethoxy-silicane, institute
The device stated has the effect that can realize tetramethoxy-silicane synthesis simultaneously and purify, fully
Embody the function of a tower multiple-effect, and at the bottom of by the isolated hydrogen chloride gas of tower top and tower
The purity of isolated tetramethoxy-silicane is above 99.9%.
The second object of the present invention is that providing a kind of utilizes above-mentioned device to prepare tetramethoxy
The method of silane, this method solves complex process, equipment throwing that traditional handicraft operation exists
Money is big, energy consumption is high, intermittent operation causes the technical problems such as unstable product quality.
In order to realize the above-mentioned purpose of the present invention, spy by the following technical solutions:
The invention provides a kind of device preparing tetramethoxy-silicane, including reactive distillation column,
Reboiler and overhead condenser；
Rectifying section, conversion zone and stripping section it is respectively from top to bottom in described reactive distillation column,
Methanol inlet port and Silicon chloride. inlet port it is provided with on outer wall residing for described conversion zone；
The bottom of described reactive distillation column is provided with on tower bottom outlet, and described tower bottom outlet and sets
It is equipped with liquid output pipe；Outside described reboiler is arranged at the bottom of the tower of described reactive distillation column, its
One end connects with described liquid output pipe, and the other end connects with described stripping section；
Described overhead condenser is arranged on the top of described reactive distillation column, and its one end is with described
The top exit connection of reactive distillation column, the other end connects overhead product recovery tube and one
The liquid return tube connected with described rectifying section.
This device preparing tetramethoxy-silicane that the present invention provides, mainly includes reaction essence
Evaporate tower, reboiler and overhead condenser；Concrete, by methanol inlet port and Silicon chloride.
After methanol and Silicon chloride. are passed in tower by inlet port, two kinds of reactants are carried out at conversion zone
React and generate tetramethoxy-silicane and byproduct hydrogen chloride gas.After sustained response, low
Boilers Silicon chloride. and hydrogen chloride can enter rectifying section with overhead reflux liquid (through tower
Liquid after the condenser cooling of top) carry out mass transfer, make the Silicon chloride. of rising be condensed into liquid,
The hydrogen chloride gas risen is input to overhead condenser from top exit, is condensed into liquid
Hydrogen chloride part as side-product extraction, part is back in tower as backflow, thus
Obtain pure hydrogen chloride liquid.High boiling substance tetramethoxy-silicane carries the methanol of part
After conversion zone enters into stripping section from top to bottom, with the tetramethoxy that evaporates in reboiler
Silane gas (derives from the liquid tetramethoxy-silicane being entered reboiler by liquid output pipe)
Carry out mass transfer, make the methanol in descending liquid gradually gasify in motor process, and derive from
Tetramethoxy-silicane in the gas of reboiler is gradually condensed into liquid, therefore, stripping section liquid
Methanol concentration in body is gradually lowered from top to bottom, after stable operation, makes the liquid at the bottom of tower
Outlet tube can obtain pure tetramethoxy-silicane liquid.
This device that the present invention provides, it is by laying multiple reaction in reactive distillation column
Section, and the physicochemical property of combine reactants carry out cooling reclaim and again boiling process, Jin Ershi
It is also carried out purifying while having showed tetramethoxy-silicane synthesis, has obtained purity from tower top and be more than
The hydrogen chloride of 99.9%, is obtaining the purity tetramethoxy-silicane liquid more than 99.9% at the bottom of tower,
Overcoming and synthesize and separate the operation complexity being separately provided and exist in prior art, equipment becomes
This high technical problem.
Optionally, described Silicon chloride. inlet port and methanol inlet port are arranged from top to bottom.
Optionally, it is provided with column plate or filler in described rectifying section and described stripping section；Described
Filler it is provided with in conversion zone.
Optionally, described column plate is bubble cap plate, valve plate or sieve plate.
Optionally, described filler is ceramic filler.
Optionally, described filler is random packing.
Optionally, the chilling temperature of described overhead condenser is not higher than hydrogen chloride under tower top pressure
Boiling point.
Optionally, the temperature of the steam in described reboiler is input to described reactive distillation column is not
Less than the boiling point of tetramethoxy-silicane under tower bottom pressure.
Optionally, the cooling medium in described overhead condenser is freon, liquefied ammonia, freezing
Saline or ethylene.
A kind of method utilizing above-mentioned device to prepare tetramethoxy-silicane, comprises the following steps:
1), Silicon chloride. and methanol are passed through Silicon chloride. inlet port and methanol inlet port respectively
It is passed in reactive distillation column so that it is react, obtains tetramethoxy-silicane and hydrogen chloride；
2), overhead condenser and the temperature of reboiler are controlled so that carry out in reactive distillation column
Stable reaction, and reclaim hydrogen chloride liquid from overhead product recovery tube, return from liquid output pipe
Receive tetramethoxy-silicane liquid.
In conjunction with the preparation method of this tetramethoxy-silicane that above-mentioned device provides, will synthesis
Reaction and separating-purifying unite two into one, and complicated process simplification can be reduced equipment investment,
Reduce operating cost.Additionally, the method energy consumption is low, reaction heat can be used for rectification and separate,
Reaction institute calorific requirement can directly be provided by reboiler, it is not necessary to additionally additional heat；And react
Speed is fast, can form gas phase reaction.
Compared with prior art, the invention have the benefit that
(1) synthesis and the separation of tetramethoxy-silicane, is achieved by a reactive distillation column
Purification operations, decreases the input of equipment while simplifying operating process, have a tower
The function of multiple-effect.
(2), by the operation of rectification and stripping, the purity pair higher than 99.9% has been obtained
Product hydrogen chloride liquid and the purity tetramethoxy-silicane liquid higher than 99.9%.
(3), at the highly purified tetramethoxy-silicane of extraction at the bottom of tower, simultaneously high at overhead extraction
The dry hydrogen chloride liquid of purity, it is achieved that extraction product and side-product in same equipment,
And eliminate rectification and purification workshop section numerous and diverse in prior art.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, with
Lower the accompanying drawing used required in embodiment or description of the prior art will be briefly described.
Fig. 1 is the structural representation of the device preparing tetramethoxy-silicane that the present invention carries.
Reference:
101-reactive distillation column；102-reboiler；103-overhead condenser；104-rectifying section；
105-conversion zone；106-stripping section；107-Silicon chloride. inlet port；108-methanol inlet port；
109-top exit；110-liquid return tube；111-tower bottom outlet；112 liquid output pipes.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but this
Skilled person is it will be appreciated that the following example is merely to illustrate the present invention, and should not regard
For limiting the scope of the present invention.Unreceipted actual conditions person in embodiment, according to normal condition
Or the condition of manufacturer's suggestion is carried out.Agents useful for same or instrument unreceipted production firm person, all
For the conventional products that can be obtained by commercially available purchase.
It addition, in the description of invention, it should be noted that term " " center ", " on ",
The orientation of the instruction such as D score, "left", "right", " vertically ", " level ", " interior ", " outward "
Or position relationship is based on orientation shown in the drawings or position relationship, it is for only for ease of description
The present invention and simplification describe rather than indicate or imply that the device of indication or element must have
Specific orientation, with specific azimuth configuration and operation, therefore it is not intended that to the present invention
Restriction.
In describing the invention, it should be noted that unless otherwise clear and definite regulation and limit
Fixed, term " is installed ", " being connected ", " connection " should be interpreted broadly, for example, it may be
Fixing connection, it is also possible to be to removably connect, or be integrally connected；Can be to be mechanically connected,
It can also be electrical connection；Can be to be joined directly together, it is also possible to be indirectly connected to by intermediary,
It can be the connection of two element internals.For the ordinary skill in the art, may be used
Above-mentioned term concrete meaning in the present invention is understood with concrete condition.
Embodiment 1
Refer to Fig. 1, embodiments provide a kind of dress preparing tetramethoxy-silicane
Put, including reactive distillation column 101, reboiler 102 and overhead condenser 103；Described reaction
Rectifying section 104, conversion zone 105 and stripping section 106 it is respectively from top to bottom in rectifying column 101,
It is provided with methanol inlet port 108 on outer wall residing for described conversion zone 105 and Silicon chloride. enters
Entrance 107；The bottom of described reactive distillation column 101 is provided with tower bottom outlet 111, and described
Liquid output pipe 112 it is provided with on tower bottom outlet 111；Described reboiler 102 is arranged on institute
Outside stating at the bottom of the tower of reactive distillation column 101, its one end connects with described liquid output pipe 112,
The other end connects with described stripping section 106；Described overhead condenser 103 be arranged on described instead
Answer the top of rectifying column 101, its one end and the top exit 109 of described reactive distillation column 101
Connection, the other end connect have an overhead product recovery tube and one connect with described rectifying section 104
Liquid return tube 110.
This device preparing tetramethoxy-silicane that the present invention provides, mainly includes reaction essence
Evaporate tower 101, reboiler 102 and overhead condenser 103；Concrete, by methanol inlet port
108 and after methanol and Silicon chloride. is passed in tower by Silicon chloride. inlet port 107, two kinds
Reactant carries out reacting and generate tetramethoxy-silicane and side product chlorinated at conversion zone 105
Hydrogen.After sustained response, low-boiling point material Silicon chloride. and hydrogen chloride can enter rectification
Section 104 passes with overhead reflux liquid (liquid after overhead condenser 103 cools down)
Matter, makes the Silicon chloride. of rising be condensed into liquid and decline along tower, the hydrogen chloride gas of rising
Body is input to overhead condenser 103 from top exit, is condensed into the hydrogen chloride portion of liquid
Being allocated as side-product extraction, part is back in tower as backflow, thus obtains pure
Hydrogen chloride liquid.High boiling substance tetramethoxy-silicane carries the methanol of part from conversion zone
After 105 enter into stripping section 106 from top to bottom, with the tetramethyl that evaporates in reboiler 102
TMOS gas (derives from the liquid four being entered reboiler 102 by liquid output pipe 112
Methoxy silane) carry out mass transfer, make the gradually gas in motor process of the methanol in descending liquid
Change, and derive from the tetramethoxy-silicane in the gas of reboiler 102 and be gradually condensed into liquid,
Therefore, the methanol concentration in stripping section 106 liquid is gradually lowered from top to bottom, stable operation
After, pure tetramethoxy-silicane liquid can be obtained at the liquid output pipe 112 made at the bottom of tower.
This device that the present invention provides, it is by laying multiple reactions in reactive distillation column 101
Section 105, and the physicochemical property of combine reactants carry out cooling reclaim and again boiling process, enter
And be also carried out purifying while achieving tetramethoxy-silicane synthesis, obtain purity from tower top
Hydrogen chloride liquid more than 99.9%, is obtaining the purity tetramethoxy more than 99.9% at the bottom of tower
Silane liquid, overcomes and synthesizes and separate the operation being separately provided and exist in prior art again
Miscellaneous, that equipment cost is high technical problem.
On the basis of above-described embodiment, in order to improve this dress preparing tetramethoxy-silicane
Put conversion ratio, make refining effect more preferably simultaneously, it is preferred that in further technical scheme
In, this device is carried out defined below, specifically refer to embodiment 2-3.
Embodiment 2
Refer to Fig. 1, on the basis of embodiment 1, it is preferred that described Silicon chloride.
Inlet port 107 and methanol inlet port 108 are arranged from top to bottom；
Owing to the boiling point of Silicon chloride. is 57.6 DEG C, less than the boiling point (64.7 DEG C) of methanol；Institute
With select two kinds of reactants are passed through in tower position time, it then follows low-boiling point material upper,
And high boiling substance under principle；Two kinds of reactants are after conversion zone 105 reacts, it is simple to
Low-boiling point material enters rectifying section 104, and high boiling substance methanol is easy in company with product four methoxy
Base silane enters stripping section 106 in the lump.Therefore, in the present embodiment, it is preferred that tetrachloro
SiClx inlet port 107 and methanol inlet port 108 are arranged from top to bottom, specifically refer to Fig. 1.
Further, it is provided with column plate in described rectifying section 104 and described stripping section 106；
It is provided with filler in described conversion zone 105；Described column plate be bubble cap plate, valve plate or
Sieve plate；Described filler is ceramic filler or random packing.
Response locations different in tower fills different media, fully to realize rectification and to carry
Evaporate effect.Further, since filling surface is long-pending big, it is more beneficial for reacting and quickly carries out, therefore,
It is preferably provided with filler at conversion zone 105.Concrete, at rectifying section 104 and stripping section 106
Column plate is set, column plate can with so that the contact of two kinds of fluid in close, carry out biphase between matter hand over
Change, to reach the purpose of separation of liquid mixtures or components of gas mixtures.Column plate is optional
Type includes: bubble cap plate, valve plate or sieve plate etc..Meanwhile, set at conversion zone 105
Put filler；Such as ceramic filler or random packing；Ceramic filler have efficiency high,
Blood pressure lowering is low, treating capacity is big, liquid holdup is little, enlarge-effect is inconspicuous, the big grade one of operating flexibility
Number of advantages.Meanwhile, random packing also possesses low pressure drop, high flux, liquid distribution
The excellent combination properties such as energy is good, mass-transfer efficiency is high, operating flexibility is big.Both are all suitable as
Filler for conversion zone 105.
The embodiment of the present invention provide the device preparing tetramethoxy-silicane, by tower not
Same conversion zone 105 selects to arrange column plate and wire feeding, and then improves gas-liquid separation effect,
Preferably to embody the effect of mass transfer, simultaneously by arranging Silicon chloride. inlet port 107 and first
The position relationship of alcohol inlet port 108 improves the conversion ratio of whole reactive distillation, it addition, more excellent
Choosing, it is passed through reactant steam at Silicon chloride. inlet port 107 and methanol inlet port 108,
To realize the reaction conversion ratio of 100%.
Embodiment 3
Refer to Fig. 1, on the basis of embodiment 2, it is preferred that described overhead condensation
The chilling temperature of device 103 is not higher than-86 DEG C (boiling temperature of hydrogen chloride under normal pressure)；
Due to the byproduct hydrogen chloride gas in stage of rectification, mainly Silicon chloride. and generation
Flow to tower top, so, during cooling, the cooling temperature of overhead condenser 103 will be stated
-86 DEG C should be not higher than；So that all gas is all condensed into liquid, after stable operation,
Partial oxidation hydrogen liquid is collected as side-product, and part continues to pass in being then back to tower
Matter.It addition, in more preferred embodiment, the two kinds of reactants entered in tower are carried out
, there is bigger pressure in pressurized treatments, in tower, the boiling point of all of material all can raise in tower,
And then it is real to facilitate overhead condenser 103 and reboiler 102 to get final product the most at a higher temperature
Now condense and produce the effect of steam, convenient operation.
Further, the steaming in described reboiler 102 is input to described reactive distillation column 101
The temperature of vapour is not less than 122 DEG C；In the reaction starting stage, the most not up to during steady statue,
Containing carrying a certain amount of methanol from the tetramethoxy-silicane of tower bottom outlet 111 output,
After this liquid is heated by reboiler 102, tetramethoxy-silicane and methanol are all converted into gaseous state
(i.e. the temperature of mixed vapour is at ambient pressure higher than the boiling temperature of tetramethoxy-silicane
-122 DEG C) and be input in tower, contact with descending liquid tetramethoxy-silicane and methanol
And after mass transfer, descending liquid methanol is all converted to gaseous state also under the effect of high-temperature steam
The up ginseng that continues is reacted, and up gaseous state tetramethoxy-silicane is condensed and liquefies and then obtain pure
Degree is more than the liquid tetramethoxy-silicane of 99.9% and directly exports also from liquid output pipe 112
Collected.And then achieve the preparation of high-purity tetramethoxy-silicane.Further, in order to
Reduce the cost of cooling, and embody the effect of environmental protection, in described overhead condenser 103
Cooling medium is freon, liquefied ammonia, chilled brine or ethylene.
It is pointed out that in FIG, the direction shown in arrow is that air-liquid or gas-liquid are mixed
The flow direction of compound, for product tetramethoxy-silicane and the collection of side-product hydrogen chloride liquid
Installation drawing 1 does not shows that, as long as it should be appreciated by those skilled in the art that and meeting accordingly
Condition of storage, uses the product collecting device that tradition is conventional.
Embodiment 4
Present invention also offers a kind of device utilizing above-described embodiment and prepare tetramethoxy-silicane
Method, comprise the following steps:
S1: Silicon chloride. and methanol are passed through Silicon chloride. inlet port and methanol inlet port respectively
It is passed in reactive distillation column so that it is react, obtains tetramethoxy-silicane and hydrogen chloride；
S2: control overhead condenser and the temperature of reboiler so that carry out in reactive distillation column
Stable reaction, and reclaim hydrogen chloride liquid from overhead product recovery tube, return from liquid output pipe
Receive tetramethoxy-silicane liquid.
Should be understood that stable reaction refers in reactive distillation column, two kinds of reactant reactions one section
After time, various materials are at different conversion zones (rectifying section, stripping section and conversion zone)
Stable state is formed, i.e. at tower top extraction hydrogen chloride liquid after mass transfer；And at the bottom of tower
Extraction tetramethoxy-silicane liquid.
By controlling the temperature of overhead condenser so that tower top enters the hydrogen chloride gas of condenser
Body is all condensed into liquid rear portion as hydrogen chloride product extraction, and remainder is from rectification
Section overhead reflux flows downward to Ta Nei and along rectifying section, runs into conversion zone in flow process
After the hydrogen chloride gas containing Silicon chloride. produced, owing to hydrogen chloride boiling point is less than Silicon chloride.
Boiling point, the Silicon chloride. in gas is gradually condensed into downward liquid flow, and hydrogen chloride liquid is subject to
Thermal evaporation becomes gas to flow up, the hydrogen chloride gas in tower top enters the gas of condenser
Silicon chloride. concentration in body is of a sufficiently low, and hydrogen chloride content is sufficiently high；After stable operation
(sustained response in tower, each phase mass transfer is stable), exports pure chlorination by overhead condenser
Hydrogen liquid.
By controlling the temperature of reboiler, make to enter at the bottom of tower the tetramethoxy-silicane gas of reboiler
Changing, the tetramethoxy-silicane after gasification enters in tower bottom stripping section, produces with conversion zone
The tetramethoxy-silicane liquid containing methanol contact in stripping section, due to tetramethoxy
The boiling point of silane is higher than methanol, and the methanol in liquid gradually flashes to gas and flows up, gas
Tetramethoxy-silicane in body is gradually condensed into downward liquid flow, finally makes to enter at the bottom of tower
Liquid in methanol content of a sufficiently low, and tetramethoxy-silicane content is sufficiently high.Treat stable
After operation, by exporting pure tetramethoxy-silicane liquid at the bottom of tower.
After measured, this device preparing tetramethoxy-silicane that the embodiment of the present invention provides with
And the purity of byproduct hydrogen chloride that method obtains is more than 99.9%；The tetramethoxy-silicane obtained
The purity of alkane is also greater than 99.9%.
To sum up, this devices and methods therefor preparing tetramethoxy-silicane that the present invention provides,
This device is totally made up of reactive distillation column, reboiler and overhead condenser, wherein reacts essence
Evaporating tower and be divided into three sections, interlude is conversion zone, and epimere is rectifying section, and hypomere is stripping section.
Wherein, silicon tetrachloride vapor is reacted at the conversion zone of reactive distillation column with methanol steam,
Purify hydrogen chloride gas at rectifying section, purify tetramethoxy-silicane at stripping section.
At the highly purified tetramethoxy-silicane of extraction at the bottom of tower, (purity is more than the method simultaneously
99.9%), at the highly purified dry hydrogen chloride of overhead extraction (99.9%), it is achieved that same
Extraction product and side-product in equipment, and eliminate numerous and diverse rectification and purification workshop section, and then
Reduce equipment investment and manual operation cost.The method have investment low, simple to operate,
The technique effect that reaction rate is fast, energy consumption is low.Meanwhile, other methoxyl group halosilanes are being prepared
And during the close silane coupler of technique, the method is the most applicable.
Although illustrate and describing the present invention with specific embodiment, but it will be appreciated that
May be made that without departing from the spirit and scope of the present invention many other change and
Amendment.It is, therefore, intended that include in the following claims belonging in the scope of the invention
All such changes and modifications.
Claims (7)
1. the method preparing tetramethoxy-silicane, it is characterised in that comprise the following steps:
1), use a kind of device preparing tetramethoxy-silicane, Silicon chloride. and methanol are divided
It is not passed in reactive distillation column by Silicon chloride. inlet port and methanol inlet port so that it is enter
Row reaction, obtains tetramethoxy-silicane and hydrogen chloride；
2), overhead condenser and the temperature of reboiler are controlled so that carry out in reactive distillation column
Stable reaction, and reclaim hydrogen chloride liquid from overhead product recovery tube, return from liquid output pipe
Receive tetramethoxy-silicane liquid；
Wherein, the device preparing tetramethoxy-silicane includes reactive distillation column, reboiler and tower
Top condenser；
Rectifying section, conversion zone and stripping section it is respectively from top to bottom in described reactive distillation column,
Methanol inlet port and Silicon chloride. inlet port it is provided with on outer wall residing for described conversion zone；
The bottom of described reactive distillation column is provided with on tower bottom outlet, and described tower bottom outlet and sets
It is equipped with liquid output pipe；Outside described reboiler is arranged at the bottom of the tower of described reactive distillation column, its
One end connects with described liquid output pipe, and the other end connects with described stripping section；
Described overhead condenser is arranged on the top of described reactive distillation column, and its one end is with described
The top exit connection of reactive distillation column, the other end connects overhead product recovery tube and one
The liquid return tube connected with described rectifying section；
Wherein, described Silicon chloride. inlet port and methanol inlet port are arranged from top to bottom；
It is provided with column plate or filler in described rectifying section and described stripping section；In described conversion zone
It is provided with filler.
The method preparing tetramethoxy-silicane the most according to claim 1, its feature exists
In, described column plate is bubble cap plate, valve plate or sieve plate.
The method preparing tetramethoxy-silicane the most according to claim 1, its feature exists
In, described filler is ceramic filler.
The method preparing tetramethoxy-silicane the most according to claim 1, its feature exists
In, described filler is random packing.
5. according to the method preparing tetramethoxy-silicane described in any one of claim 1-4,
It is characterized in that, the chilling temperature of described overhead condenser is not higher than hydrogen chloride under tower top pressure
Boiling point.
The method preparing tetramethoxy-silicane the most according to claim 5, its feature exists
In, described reboiler is input to the temperature of the steam in described reactive distillation column and is not less than at the bottom of tower
The boiling point of tetramethoxy-silicane under pressure.
The method preparing tetramethoxy-silicane the most according to claim 6, its feature exists
In, the cooling medium in described overhead condenser is freon, liquefied ammonia, chilled brine or second
Alkene.
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| CN105348115B (en) * | 2015-12-23 | 2017-10-20 | 山西翔宇化工有限公司 | A kind of reaction again of rubber antioxidant substandard products and purification processes device |
| CN106565516B (en) * | 2016-11-14 | 2019-08-13 | 成都惠恩精细化工有限责任公司 | A kind of chain alkyl formamide, preparation method and formylated rectifier unit |
| CN109748931B (en) * | 2019-02-18 | 2020-04-07 | 苏州金宏气体股份有限公司 | Preparation method and production system of high-purity ethyl orthosilicate |
| CN110357766A (en) * | 2019-06-05 | 2019-10-22 | 南京康立瑞生物科技有限公司 | It is a kind of to prepare chloromethyl ether compound preparation process and its Preparation equipment |
| CN110559678B (en) * | 2019-10-21 | 2024-02-27 | 无锡赫利邦化工科技有限公司 | Rectifying tower for synthesizing and separating polymethoxy dimethyl ether and application method thereof |
| CN111974018B (en) * | 2020-09-02 | 2022-07-12 | 中国林业科学研究院林产化学工业研究所 | Efficient condensation, collection and separation method for biomass pyrolysis gas |
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