CN104437295A - Device and method for preparing tetramethoxysilane - Google Patents
Device and method for preparing tetramethoxysilane Download PDFInfo
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- CN104437295A CN104437295A CN201410816621.7A CN201410816621A CN104437295A CN 104437295 A CN104437295 A CN 104437295A CN 201410816621 A CN201410816621 A CN 201410816621A CN 104437295 A CN104437295 A CN 104437295A
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- reactive distillation
- tetramethoxy
- silicane
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- 238000000034 method Methods 0.000 title claims abstract description 28
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 title abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 118
- 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 44
- 239000005049 silicon tetrachloride Substances 0.000 claims abstract description 33
- 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 claims abstract description 32
- 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 37
- 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 22
- 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
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- 239000012267 brine Substances 0.000 claims description 3
- 239000002826 coolant Substances 0.000 claims description 3
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 3
- 230000008569 process Effects 0.000 abstract description 11
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 22
- 230000015572 biosynthetic process Effects 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- 239000006227 byproduct Substances 0.000 description 11
- 238000000605 extraction Methods 0.000 description 11
- 230000000694 effects Effects 0.000 description 9
- 239000000376 reactant Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 239000004567 concrete Substances 0.000 description 6
- 238000000746 purification Methods 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 230000004044 response Effects 0.000 description 4
- 239000012043 crude product Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- 230000002459 sustained effect Effects 0.000 description 3
- 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
- 238000002309 gasification Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001143 conditioned effect 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
- 238000011049 filling Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000010574 gas phase reaction Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- -1 methoxyl group Chemical group 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
- 230000036632 reaction speed Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- JICSOOZUSBLTQQ-UHFFFAOYSA-N tetrachlorosilane hydrochloride Chemical compound Cl.Cl[Si](Cl)(Cl)Cl JICSOOZUSBLTQQ-UHFFFAOYSA-N 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
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- 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 a device and a method for preparing tetramethoxysilane and relates to the field of tetramethoxysilane preparation. The device comprises a reactive distillation tower, a reboiler and an overhead condenser; a rectification section, a reaction section and a stripping section are arranged in the reactive distillation tower from top to bottom; a methanol inlet and a silicon tetrachloride inlet are formed in the outer wall of the reaction section; a tower bottom outlet is formed in the bottom of the reactive distillation tower, and a liquid outputting pipe is arranged at the tower bottom outlet; the reboiler is arranged outside the bottom of the reactive distillation tower, and one end of the reboiler is communicated with a tower bottom outlet pipe, while the other end of the reboiler is communicated with the stripping section; the overhead condenser is arranged at the top of the reactive distillation tower, and one end of the overhead condenser is communicated with a top outlet of the reactive distillation tower, while the other end of the overhead condenser is connected with a top product recovery pipe and a liquid return pipe communicated with the rectification section. The device is integrated with reaction and separation devices, and therefore, the complex process is simplified, and the equipment investment and the operating cost are reduced.
Description
Technical field
The present invention relates to tetramethoxy-silicane preparation field, in particular to a kind of device and method preparing tetramethoxy-silicane.
Background technology
Tetramethoxy-silicane can be used as the insulating materials in the fields such as organosilicon synthesis, heat resistant paint manufacture, adhesive, electronics industry, is also the important raw and processed materials of optical glass inorganic agent and coagulating agent etc.; It is widely used, so its synthesis receives the concern of chemical industry always.
Traditional synthetic method is by silicon tetrachloride and the direct liquid phase reactor of methyl alcohol, and by controlling the burden control reaction speed of silicon tetrachloride and methyl alcohol, the tetramethoxy-silicane of generation needs the purity that can be reached more than 99% by further rectification and purification technique.This kind of traditional tetramethoxy-silicane synthetic method its be divided into two operating processes, being first the Reactive Synthesis stage, is secondly carried out by the crude product of synthesis purifying stage of (being namely separated).In concrete Chemical Manufacture, Reactive Synthesis and separating-purifying two kinds operation are usually carried out respectively in the independent equipment of two classes; Namely first utilize consersion unit to synthesize crude product, and then crude product is input in another equipment for purifying carries out purification processes.
Therefore, traditional prepares tetramethoxy-silicane equipment, because the equipment of synthesis and separating-purifying is independent setting, the problem such as therefore there is whole preparation technology's complicated operation, long flow path, equipment investment is large, yield is low, energy consumption is high, and then tetramethoxy-silicane combined coefficient also can be caused low, price, up to more than 10,000 yuan per ton, limits application, and causes downstream product cost increase.
In view of this, special proposition the present invention.
Summary of the invention
The first object of the present invention is to provide a kind of device preparing tetramethoxy-silicane, described device has the effect that can realize tetramethoxy-silicane synthesis simultaneously and purify, fully demonstrate the function of a tower multiple-effect, and by the purity of isolated tetramethoxy-silicane at the bottom of the isolated hydrogen chloride gas of tower top and tower all higher than 99.9%.
The second object of the present invention is to provide a kind of method utilizing above-mentioned device to prepare tetramethoxy-silicane, this method solves the complex process of traditional handicraft operation existence, equipment investment is large, energy consumption is high, intermittent operation causes the technical problems such as unstable product quality.
In order to realize above-mentioned purpose of the present invention, spy by the following technical solutions:
The invention provides a kind of device preparing tetramethoxy-silicane, comprise reactive distillation column, reboiler and overhead condenser;
Be respectively rectifying section, conversion zone and stripping section from top to bottom in described reactive distillation column, the outer wall residing for described conversion zone be provided with methyl alcohol inlet port and silicon tetrachloride inlet port;
The bottom of described reactive distillation column is provided with tower bottom outlet, and described tower bottom outlet is provided with liquid output pipe; Described reboiler is arranged on outside at the bottom of the tower of described reactive distillation column, and its one end is communicated with described liquid output pipe, and the other end is communicated with described stripping section;
Described overhead condenser is arranged on the top of described reactive distillation column, and its one end is communicated with the top exit of described reactive distillation column, and the other end is connected with overhead product recovery tube and a liquid return tube be communicated with described rectifying section.
This device preparing tetramethoxy-silicane provided by the invention, mainly comprises reactive distillation column, reboiler and overhead condenser; Concrete, methyl alcohol and silicon tetrachloride are passed into after in tower by methyl alcohol inlet port and silicon tetrachloride inlet port, two kinds of reactants carry out reacting at conversion zone and generate tetramethoxy-silicane and byproduct hydrogen chloride gas.After sustained response, low-boiling point material silicon tetrachloride and hydrogen chloride can enter rectifying section and overhead reflux liquid (through the cooled liquid of overhead condenser) carries out mass transfer, the silicon tetrachloride of rising is made to be condensed into liquid, the hydrogen chloride gas risen is input to overhead condenser from top exit, be condensed into the hydrogen chloride part of liquid as byproduct extraction, part is back in tower as phegma, thus obtains pure hydrogen chloride liquid.High boiling substance tetramethoxy-silicane carry part methyl alcohol enter into stripping section from top to bottom from conversion zone after, mass transfer is carried out with the tetramethoxy-silicane gas evaporated in reboiler (deriving from the liquid tetramethoxy-silicane being entered reboiler by liquid output pipe), methyl alcohol in descending liquid is gasified gradually in motion process, and the tetramethoxy-silicane derived from the gas of reboiler is condensed into liquid gradually, therefore, methanol concentration in stripping section liquid reduces from top to bottom gradually, after stable operation, pure tetramethoxy-silicane liquid can be obtained making the liquid output pipe at the bottom of tower.
This device provided by the invention, it by laying multiple conversion zone in reactive distillation column, and the physicochemical property of combine reactants carries out cooling recovery and process of boiling again, and then also purify while achieving tetramethoxy-silicane synthesis, the hydrogen chloride that purity is greater than 99.9% is obtained from tower top, at the bottom of tower, obtain the tetramethoxy-silicane liquid that purity is greater than 99.9%, overcome synthesis in prior art and arrange separately and the complicated operation of existence with being separated, the technical problem that equipment cost is high.
Optionally, described silicon tetrachloride inlet port and methyl alcohol inlet port are arranged from top to bottom.
Optionally, column plate or filler is provided with in described rectifying section and described stripping section; Filler is provided with in described 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 the boiling point of hydrogen chloride under tower top pressure.
Optionally, the temperature of steam that described reboiler is input in 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, chilled brine or ethene.
Utilize above-mentioned device to prepare a method for tetramethoxy-silicane, comprise the following steps:
1), silicon tetrachloride and methyl alcohol are passed in reactive distillation column respectively by silicon tetrachloride inlet port and methyl alcohol inlet port, make it react, obtain tetramethoxy-silicane and hydrogen chloride;
2), control the temperature of overhead condenser and reboiler, make in reactive distillation column, to carry out stable reaction, and reclaim hydrogen chloride liquid from overhead product recovery tube, reclaim tetramethoxy-silicane liquid from liquid output pipe.
In conjunction with the preparation method of this tetramethoxy-silicane that above-mentioned device provides, synthetic reaction and separating-purifying are united two into one, by the process simplification of complexity, equipment investment can be reduced, reduce operating cost.In addition, the method energy consumption is low, reaction heat can be used for rectifying and be separated, and reaction institute calorific requirement can directly be provided by reboiler, without the need to other additional heat; And reaction rate is fast, can form gas-phase reaction.
Compared with prior art, beneficial effect of the present invention is:
(1), by a reactive distillation column achieve synthesis and the separating-purifying operation of tetramethoxy-silicane, decrease the input of equipment while simplifying operating process, there is the function of a tower multiple-effect.
(2), by rectifying and propose the operation of heating up in a steamer, obtain purity higher than 99.9% byproduct hydrogen chloride liquid and purity higher than 99.9% tetramethoxy-silicane liquid.
(3), at the bottom of tower the highly purified tetramethoxy-silicane of extraction, simultaneously at the highly purified dry hydrogen chloride liquid of overhead extraction, achieve extraction product and byproduct 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 in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below.
Fig. 1 is the structural representation preparing the device of tetramethoxy-silicane that the present invention carries.
Reference numeral:
101-reactive distillation column; 102-reboiler; 103-overhead condenser; 104-rectifying section; 105-conversion zone; 106-stripping section; 107-silicon tetrachloride inlet port; 108-methyl alcohol 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 it will be understood to those of skill in the art that the following example only for illustration of the present invention, and should not be considered as limiting the scope of the invention.Unreceipted actual conditions person in embodiment, the condition of conveniently conditioned disjunction manufacturer suggestion is carried out.Agents useful for same or the unreceipted production firm person of instrument, be and can buy by commercially available the conventional products obtained.
In addition, in the description of invention, it should be noted that, orientation or the position relationship of the instruction such as term " " center ", " on ", D score, "left", "right", " vertically ", " level ", " interior ", " outward " they be based on orientation shown in the drawings or position relationship; be only the present invention for convenience of description and simplified characterization; instead of instruction or imply the device of indication or element must have specific orientation, with specific azimuth configuration and operation, therefore can not be interpreted as limitation of the present invention.
In describing the invention, it should be noted that, unless otherwise clearly defined and limited, term " installation ", " being connected ", " connection " should be interpreted broadly, and such as, can be fixedly connected with, also can be removably connect, or connect integratedly; Can be mechanical connection, also can be electrical connection; Can be directly be connected, also indirectly can be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, concrete condition above-mentioned term concrete meaning in the present invention can be understood.
Embodiment 1
Please refer to Fig. 1, embodiments provide a kind of device preparing tetramethoxy-silicane, comprise reactive distillation column 101, reboiler 102 and overhead condenser 103; Be respectively rectifying section 104, conversion zone 105 and stripping section 106 in described reactive distillation column 101 from top to bottom, the outer wall residing for described conversion zone 105 be provided with methyl alcohol inlet port 108 and silicon tetrachloride inlet port 107; The bottom of described reactive distillation column 101 is provided with tower bottom outlet 111, and described tower bottom outlet 111 is provided with liquid output pipe 112; Described reboiler 102 is arranged on outside at the bottom of the tower of described reactive distillation column 101, and its one end is communicated with described liquid output pipe 112, and the other end is communicated with described stripping section 106; Described overhead condenser 103 is arranged on the top of described reactive distillation column 101, and its one end is communicated with the top exit 109 of described reactive distillation column 101, and the other end is connected with overhead product recovery tube and a liquid return tube 110 be communicated with described rectifying section 104.
This device preparing tetramethoxy-silicane provided by the invention, mainly comprises reactive distillation column 101, reboiler 102 and overhead condenser 103; Concrete, methyl alcohol and silicon tetrachloride are passed into after in tower by methyl alcohol inlet port 108 and silicon tetrachloride inlet port 107, two kinds of reactants carry out reacting at conversion zone 105 and generate tetramethoxy-silicane and byproduct hydrogen chloride gas.After sustained response, low-boiling point material silicon tetrachloride and hydrogen chloride can enter rectifying section 104 and carry out mass transfer with overhead reflux liquid (through the cooled liquid of overhead condenser 103), the silicon tetrachloride of rising is made to be condensed into liquid and to decline along in tower, the hydrogen chloride gas risen is input to overhead condenser 103 from top exit, be condensed into the hydrogen chloride part of liquid as byproduct extraction, part is back in tower as phegma, thus obtains pure hydrogen chloride liquid.High boiling substance tetramethoxy-silicane carry part methyl alcohol enter into stripping section 106 from top to bottom from conversion zone 105 after, mass transfer is carried out with the tetramethoxy-silicane gas evaporated in reboiler 102 (deriving from the liquid tetramethoxy-silicane being entered reboiler 102 by liquid output pipe 112), methyl alcohol in descending liquid is gasified gradually in motion process, and the tetramethoxy-silicane derived from the gas of reboiler 102 is condensed into liquid gradually, therefore, methanol concentration in stripping section 106 liquid reduces from top to bottom gradually, after stable operation, pure tetramethoxy-silicane liquid can be obtained at the liquid output pipe 112 made at the bottom of tower.This device provided by the invention, it by laying multiple conversion zone 105 in reactive distillation column 101, and the physicochemical property of combine reactants carries out cooling recovery and process of boiling again, and then also purify while achieving tetramethoxy-silicane synthesis, the hydrogen chloride liquid that purity is greater than 99.9% is obtained from tower top, the tetramethoxy-silicane liquid that purity is greater than 99.9% is obtained at the bottom of tower, overcome synthesis in prior art to arrange separately and the complicated operation of existence with being separated, the technical problem that equipment cost is high.
On the basis of above-described embodiment, in order to improve the device conversion ratio that this prepares tetramethoxy-silicane, making refining effect better simultaneously, preferably, in further technical scheme, following restriction being carried out to this device, specifically please refer to embodiment 2-3.
Embodiment 2
Please refer to Fig. 1, on the basis of embodiment 1, preferably, described silicon tetrachloride inlet port 107 and methyl alcohol inlet port 108 are arranged from top to bottom;
Boiling point due to silicon tetrachloride is 57.6 DEG C, lower than the boiling point (64.7 DEG C) of methyl alcohol; So select two kinds of reactants are passed into the position in tower time, follow low-boiling point material upper, and high boiling substance under principle; Two kinds of reactants, after conversion zone 105 reacts, are convenient to low-boiling point material and are entered rectifying section 104, and high boiling substance methyl alcohol is convenient to enter stripping section 106 in the lump in company with product tetramethoxy-silicane.Therefore, in the present embodiment, preferably, silicon tetrachloride inlet port 107 and methyl alcohol inlet port 108 are arranged from top to bottom, specifically please refer to Fig. 1.
Further, column plate is provided with in described rectifying section 104 and described stripping section 106; Filler is provided with in described conversion zone 105; Described column plate is bubble cap plate, valve plate or sieve plate; Described filler is ceramic filler or random packing.
Response locations different in tower fills different media, heats up in a steamer effect fully to realize rectifying and to carry.In addition, because filling surface is long-pending large, be more conducive to reaction and carry out fast, therefore, at conversion zone 105, preferably filler is set.Concrete, arrange column plate at rectifying section 104 and stripping section 106, column plate in order to make two kinds of fluid in close contacts, can carry out the mass transter between two-phase, to reach the object of separation of liquid mixtures or components of gas mixtures.The optional type of column plate comprises: bubble cap plate, valve plate or sieve plate etc.Meanwhile, filler is set at conversion zone 105; As ceramic filler or random packing; Ceramic filler has that efficiency is high, step-down is low, treating capacity is large, liquid holdup is little, enlarge-effect is not obvious, the series of advantages such as operating flexibility is large.Meanwhile, excellent combination property that random packing also has low pressure drop, high flux, liquid-distribution property is good, mass-transfer efficiency is high, operating flexibility is large etc.Both are all suitable as the filler of conversion zone 105.
The device of what the embodiment of the present invention provided prepare tetramethoxy-silicane, select to arrange column plate and wire feeding by conversion zones 105 different in tower, and then raising gas-liquid separation effect, better to embody the effect of mass transfer, position relationship simultaneously by arranging silicon tetrachloride inlet port 107 and methyl alcohol inlet port 108 improves the conversion ratio of whole reactive distillation, in addition, preferred, reactant steam is passed into, to realize the reaction conversion ratio of 100% at silicon tetrachloride inlet port 107 and methyl alcohol inlet port 108.
Embodiment 3
Please refer to Fig. 1, on the basis of embodiment 2, preferably, the chilling temperature of described overhead condenser 103 is not higher than-86 DEG C the boiling temperature of hydrogen chloride (under normal pressures);
Due in stage of rectification, the byproduct hydrogen chloride gas of mainly silicon tetrachloride and generation flows to tower top, so, in the process of cooling, should not higher than-86 DEG C by the cooling temperature stating overhead condenser 103; To make all gas all be condensed into liquid, after stable operation, partial oxidation hydrogen liquid is collected by as byproduct, and part is then back in tower and continues mass transfer.In addition, in more preferred embodiment, pressurized treatments is carried out to the two kinds of reactants entered in tower, larger pressure is there is in tower, the boiling point of materials all in tower all can raise, and then facilitate overhead condenser 103 and reboiler 102 can realize condensation respectively at a higher temperature and produce the effect of steam, handled easily.
Further, the temperature of steam that described reboiler 102 is input in described reactive distillation column 101 is not less than 122 DEG C, in the reaction starting stage, when namely not reaching stable state, containing carrying a certain amount of methyl alcohol from the tetramethoxy-silicane that tower bottom outlet 111 exports, after this liquid is heated by reboiler 102, tetramethoxy-silicane and methyl alcohol all convert gaseous state (namely the temperature of mixed vapour is at ambient pressure higher than the boiling temperature-122 DEG C of tetramethoxy-silicane) to and are input in tower, contact with descending liquid tetramethoxy-silicane and methyl alcohol and mass transfer after, descending liquid methanol is all converted to gaseous state and the reaction of up continuation ginseng under the effect of high-temperature steam, up gaseous state tetramethoxy-silicane is condensed liquefaction and then obtain purity and be greater than the liquid tetramethoxy-silicane of 99.9% and directly export and collected from liquid output pipe 112.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, the cooling medium in described overhead condenser 103 is freon, liquefied ammonia, chilled brine or ethene.
It is to be noted, in FIG, direction shown in arrow is the flow direction of gas, liquid or gas-liquid mixture, for not shown in gathering-device Fig. 1 of product tetramethoxy-silicane and byproduct hydrogen chloride liquid, those skilled in the art should understand that, as long as meet corresponding condition of storage, adopt the product-collecting equipment that tradition is conventional.
Embodiment 4
Present invention also offers a kind of method utilizing the device of above-described embodiment to prepare tetramethoxy-silicane, comprise the following steps:
S1: silicon tetrachloride and methyl alcohol are passed in reactive distillation column respectively by silicon tetrachloride inlet port and methyl alcohol inlet port, make it react, obtain tetramethoxy-silicane and hydrogen chloride;
S2: the temperature controlling overhead condenser and reboiler, makes to carry out stable reaction in reactive distillation column, and reclaims hydrogen chloride liquid from overhead product recovery tube, reclaim tetramethoxy-silicane liquid from liquid output pipe.
Should understand, stable reaction refers in reactive distillation column, after two kinds of reactant reaction a period of times, various material forms stable state after different conversion zone (rectifying section, stripping section and conversion zone) mass transfers, namely at a tower top extraction hydrogen chloride liquid; And at the bottom of tower an extraction tetramethoxy-silicane liquid.
By controlling the temperature of overhead condenser, the hydrogen chloride gas making tower top enter condenser is all condensed into liquid rear portion as the extraction of hydrogen chloride product, remainder is from rectifying section overhead reflux to Ta Nei and flow downward along rectifying section, run in flow process conversion zone produce containing silicon tetrachloride hydrogen chloride gas after, because hydrogen chloride boiling point is lower than silicon tetrachloride boiling point, silicon tetrachloride in gas is condensed into downward liquid flow gradually, hydrogen chloride liquid is heated and flashes to gas and upwards flow, the silicon tetrachloride concentration entered through tower top in the hydrogen chloride gas in the gas of condenser is enough low, and hydrogen chloride content is enough high, after stable operation (in tower sustained response, each phase mass transfer stablize), export pure hydrogen chloride liquid by overhead condenser.
By controlling the temperature of reboiler, make the tetramethoxy-silicane gasification entering reboiler at the bottom of tower, tetramethoxy-silicane after gasification enters in tower bottom stripping section, contact in stripping section with the tetramethoxy-silicane liquid containing methyl alcohol that conversion zone produces, because the boiling point of tetramethoxy-silicane is higher than methyl alcohol, methyl alcohol in liquid flashes to gas gradually and upwards flows, tetramethoxy-silicane in gas is condensed into downward liquid flow gradually, finally make the methanol content of the liquid entered at the bottom of tower enough low, and tetramethoxy-silicane content is enough high.After stable operation, by exporting pure tetramethoxy-silicane liquid at the bottom of tower.
After measured, the embodiment of the present invention provide this prepare tetramethoxy-silicane device and the purity of byproduct hydrogen chloride that obtains of method be greater than 99.9%; The purity of the tetramethoxy-silicane obtained also is greater than 99.9%.
To sum up, this devices and methods therefor preparing tetramethoxy-silicane provided by the invention, this device is totally made up of reactive distillation column, reboiler and overhead condenser, wherein reactive distillation column is divided into three sections, interlude is conversion zone, and epimere is rectifying section, and hypomere is stripping section.Wherein, silicon tetrachloride vapor and methanol steam react at the conversion zone of reactive distillation column, at rectifying section purification hydrogen chloride gas, at stripping section purification tetramethoxy-silicane.
The method is the highly purified tetramethoxy-silicane of extraction (purity is greater than 99.9%) at the bottom of tower simultaneously, at the highly purified dry hydrogen chloride of overhead extraction (99.9%), achieve extraction product and byproduct in same equipment, and eliminate numerous and diverse rectification and purification workshop section, and then reduce equipment investment and manual operation cost.The method has the technique effect that investment is low, simple to operate, reaction rate is fast, energy consumption is low.Meanwhile, when preparing other methoxyl group halosilanes and the close silane coupler of technique, the method is all applicable.
Although illustrate and describe the present invention with specific embodiment, however it will be appreciated that can to make when not deviating from the spirit and scope of the present invention many other change and amendment.Therefore, this means to comprise all such changes and modifications belonged in the scope of the invention in the following claims.
Claims (10)
1. prepare the device of tetramethoxy-silicane, it is characterized in that, comprise reactive distillation column, reboiler and overhead condenser;
Be respectively rectifying section, conversion zone and stripping section from top to bottom in described reactive distillation column, the outer wall residing for described conversion zone be provided with methyl alcohol inlet port and silicon tetrachloride inlet port;
The bottom of described reactive distillation column is provided with tower bottom outlet, and described tower bottom outlet is provided with liquid output pipe; Described reboiler is arranged on outside at the bottom of the tower of described reactive distillation column, and its one end is communicated with described liquid output pipe, and the other end is communicated with described stripping section;
Described overhead condenser is arranged on the top of described reactive distillation column, and its one end is communicated with the top exit of described reactive distillation column, and the other end is connected with overhead product recovery tube and a liquid return tube be communicated with described rectifying section.
2. device according to claim 1, is characterized in that, described silicon tetrachloride inlet port and methyl alcohol inlet port are arranged from top to bottom.
3. device according to claim 1, is characterized in that, is provided with column plate or filler in described rectifying section and described stripping section; Filler is provided with in described conversion zone.
4. device according to claim 3, is characterized in that, described column plate is bubble cap plate, valve plate or sieve plate.
5. device according to claim 3, is characterized in that, described filler is ceramic filler.
6. device according to claim 3, is characterized in that, described filler is random packing.
7. the device according to any one of claim 1-6, is characterized in that, the chilling temperature of described overhead condenser is not higher than the boiling point of hydrogen chloride under tower top pressure.
8. device according to claim 7, is characterized in that, the temperature of the steam that described reboiler is input in described reactive distillation column is not less than the boiling point of tetramethoxy-silicane under tower bottom pressure.
9. device according to claim 8, is characterized in that, the cooling medium in described overhead condenser is freon, liquefied ammonia, chilled brine or ethene.
10. the device according to any one of claim 1-9 prepares a method for tetramethoxy-silicane, it is characterized in that, comprises the following steps:
1), silicon tetrachloride and methyl alcohol are passed in reactive distillation column respectively by silicon tetrachloride inlet port and methyl alcohol inlet port, make it react, obtain tetramethoxy-silicane and hydrogen chloride;
2), control the temperature of overhead condenser and reboiler, make in reactive distillation column, to carry out stable reaction, and reclaim hydrogen chloride liquid from overhead product recovery tube, reclaim tetramethoxy-silicane liquid from liquid output pipe.
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