CN209093380U - A kind of reaction tower for continuous production organosilicon - Google Patents
A kind of reaction tower for continuous production organosilicon Download PDFInfo
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- CN209093380U CN209093380U CN201821652930.5U CN201821652930U CN209093380U CN 209093380 U CN209093380 U CN 209093380U CN 201821652930 U CN201821652930 U CN 201821652930U CN 209093380 U CN209093380 U CN 209093380U
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Abstract
Originally practical to disclose a kind of reaction tower for continuous production organosilicon, including reaction tower, condenser, reboiler and controller, on the reaction tower by from top to bottom be sequentially set with exhaust outlet, inlet port and outlet port, the exhaust outlet is connected with condenser, and the reboiler is connected with reaction tower respectively by circulation port and liquid back pipe；The controller is connected with the temperature sensor in reaction tower；The utility model reacts in reaction tower generates esters of silicon acis, utilize the difference of various material boiling points, the higher esters of silicon acis of purity will be obtained after various substances separation in reaction product, while the utility model also achieves the continuous production of esters of silicon acis, substantially increases the efficiency of reaction.
Description
Technical field
The utility model relates to chemical equipment technical fields, and in particular to a kind of reaction for continuous production organosilicon
Tower.
Background technique
At present since building materials and pesticide industry are quickly grown, silester application field is constantly expanded, and enters quick hair
The duration of an exhibition.Since most domestic manufacturing enterprise is to use the higher silicon tetrachloride of purity for raw material, and this raw material is mainly derived from
Waste in polysilicon production process, thus its production influenced by polysilicon and chlorosilane enterprise it is more apparent；With the country
Demand of the market to silester increases severely, and country is to chemical industry environmental protection increasingly higher demands, it would be highly desirable to develop a kind of pollution
Small, high income, high-quality, high-efficient silester new production process；And in the various methods for preparing silester, only
Two methods of silicon powder method and silicon tetrachloride method realize industrialization, wherein with silicon tetrachloride method, (ethyl alcohol and silicon tetrachloride are carried out again
Esterification) produce silester method it is most popular, still used at home by most producers.
The Chinese utility model patent of Publication No. CN207709033U was disclosed on August 10th, 2018 a kind of prepares silicon
The reaction kettle device of acetoacetic ester, including kettle ontology and the reaction tower being arranged on kettle ontology, kettle ontology is connected to reaction tower, kettle sheet
It is provided with the first collet for being passed through steam in vitro, the lower end for reacting tower side wall is connected with the first pipe that ethyl alcohol is passed through, instead
The upper end of tower side wall is answered to be connected with the second pipe that silicon tetrachloride is passed through, the upper end of reaction tower is connected with for handling hydrogen chloride gas
The gas collector of body.The utility model enables to silicon tetrachloride that can prevent in itself and air in time and ethanol synthesis
Contact with moisture, and hydrogen chloride gas can be removed in time, improve main reaction, reduced side reaction and by-product, improve production
Object yield；Although the utility model can be realized the preparation of organosilicon, but since it is carried out instead by way of heating ethyl alcohol
It answers, therefore reaction product can only could be taken out after the ethanol synthesis in each kettle and add new reactant progress again by it
Reaction, cannot achieve the continuous production of organosilicon, therefore its production efficiency is lower；In addition, being generated due to being gap production
The process of byproduct hydrogen chloride is discontinuous, cannot collect hydrogen chloride and recycle, can only lead to and do hydrochloric acid in aqueous solution, make
At quantity of three wastes it is big, be not able to satisfy the requirement of green economy.
Summary of the invention
It is low for continuous production, the production efficiency existing in the prior art of not can be carried out, the defects such as raw material availability is low,
The utility model discloses a kind of esters of silicon acis reaction tower with continuous production ability, the utility model realizes the company of esters of silicon acis
Continuous production, not only substantially increases production efficiency, and can exclude in time reaction product, to guarantee reaction always in most
Good state substantially increases the utilization rate of reaction, improves the economic benefit of enterprise；Simultaneously as the utility model realizes
Continuous production, i.e. byproduct hydrogen chloride also can introduce process (such as chlorine for needing to consume hydrogen chloride with a certain amount of stable discharge
Silane synthesis procedure) in recycle, meet advocating for circular economy.
The utility model is achieved through the following technical solutions above-mentioned purpose:
A kind of reaction tower for continuous production organosilicon, including reaction tower, reboiler and controller, it is characterised in that:
Exhaust outlet, inlet port and outlet port are disposed on the reaction tower from top to bottom；Circulation is additionally provided on the reaction tower
Mouth and feedback outlet, the outlet end of the reboiler and input end are connected with circulation port and feedback outlet respectively.
The feed inlet includes first charging aperture and second charging aperture, is all provided in the first charging aperture and second charging aperture
Be equipped with flowmeter and regulating valve, the flowmeter and regulating valve be connected respectively with controller.
The temperature sensor and pressure sensor being connected with controller are additionally provided in the reaction tower.
The reaction tower bottom is provided with liquidometer, and regulating valve, the liquidometer and regulating valve point are provided on discharge port
It is not connected with controller.
The reboiler is Steam reboiler or conduction oil reboiler, is provided on the steam inlet of reboiler and controller
Connected heating agent regulating valve.
Multiple column plates or packing layer are additionally provided in the reaction tower.
It is connected with condenser on the exhaust outlet, the feedback outlet being connected with tower body is provided on the condenser and for arranging
The gas-guide tube of tail gas out.
It is additionally provided with the spray tube being connected with feed inlet in the reaction tower, is provided with spray head on the spray tube.
Compared with prior art, the utility model has the following beneficial effects:
1, the utility model includes reaction tower, condenser, reboiler and controller, be provided on the reaction tower first into
Material mouth and second charging aperture, reaction tower bottom are provided with discharge port and circulation port, and circulation port is connected by reboiler with feedback outlet；
The utility model is injected separately into ethyl alcohol and silicon tetrachloride into reaction tower by first charging aperture and second charging aperture, and reactant exists
It reacts in reaction tower and generates esters of silicon acis, since reaction product material is different from the boiling point of reaction raw materials, reaction is generated
Hydrogen chloride in material is directly excluded from the exhaust outlet at top, and esters of silicon acis, ethyl alcohol are then fallen with silicon tetrachloride with the state of liquid
Enter to reaction tower bottom, then entered in reboiler by circulation port, since the boiling point between above-mentioned three kinds of materials is different,
Only esters of silicon acis is liquid from the material that feedback outlet excludes, and ethyl alcohol and silicon tetrachloride are flowed back into instead with the state of gas again
Reaction is participated on the top Ying Ta, to guarantee the esters of silicon acis purity of reaction tower bottom, the esters of silicon acis that simultaneous reactions generate passes through discharging
Mouth discharge reaction tower, realizes the recycling to final products, and compared with prior art, the utility model passes through heating final products
Mode not only improved the purity of product, but also being carried out continuously for reaction is realized, to substantially increase production efficiency；Simultaneously originally
Constantly esters of silicon acis is discharged by discharge port while producing esters of silicon acis for utility model, to guarantee in tower body and aggregate tank
Silicic acid ester content all-the-time stable avoids in lower level and inhibits even to reverse generation esters of silicon acis because silicic acid ester content increases
Reaction also reduce the content of impurity in product to substantially increase the utilization rate of raw material, improve the economic effect of enterprise
Benefit.
2, pressure sensor and temperature sensor, first charging aperture and the second charging are provided on the tower body of the utility model
Mouth is provided with flowmeter and regulating valve, monitors in real time, while controlling the additive amount of raw material, makes to the reaction process in tower body
Reaction in tower body is in optimum state always, to improve the utilization rate of raw material and the yield of finished product.
3, the reaction tower bottom of the utility model is provided with liquidometer, and the adjusting being connected with controller is provided on discharge port
Valve opens regulating valve after esters of silicon acis reaches discharge amount by the silicic acid ester content in liquidometer real-time monitoring aggregate tank, from
And obtain esters of silicon acis finished product, guarantee aggregate tank in silicic acid ester content stabilization, not only realized esters of silicon acis it is continuous recycle but also can
It avoids inhibiting the progress reacted because esters of silicon acis is excessive, improves production efficiency.
4, the reboiler of the utility model is Steam reboiler or conduction oil reboiler, is provided with and controls on the reboiler
The connected heating agent regulating valve of device processed enters the quantity of steam in reboiler by the control of heating agent regulating valve, thus according to being input to
Inventory and environment temperature are adjusted flexibly the control temperature of reboiler, guarantee to vaporize the impurity such as ethyl alcohol, hydrogen chloride in material
Discharge, and then ensure to produce the quality of product.
5, it is provided with column plate or packing layer in the tower body of the utility model, extends silicon tetrachloride and ethyl alcohol stops in tower body
The time is stayed, to keep raw material reaction more abundant, improves the utilization rate of raw material.
6, it is provided with condenser on the exhaust outlet of the utility model, the feedback outlet being connected with tower body is provided on condenser,
Using the difference of the material boiling points such as hydrogen chloride and ethyl alcohol, recycled by cooling by HCl separation, and to materials such as ethyl alcohol
It utilizes, and hydrogen chloride then passes through gas-guide tube and enters using it as in the equipment that raw material is produced, and has both improved the utilization of raw material
Rate, while by, using the environmental discharge pressure for reducing enterprise, improving the economic benefit of enterprise to hydrogen chloride.
7, the utility model is provided with the first spray tube and the second spray tube, the first spray tube and the second spray in reaction tower
It is provided with spray head in shower pipe, guarantees that reactant can be sufficiently mixed, to accelerate the process of reaction, improves the production effect of equipment
Rate.
Detailed description of the invention
Fig. 1 is 1 structural schematic diagram of the utility model embodiment；
Fig. 2 is 1 feed inlet distribution map of the utility model embodiment；
Fig. 3 is 2 structural schematic diagram of the utility model embodiment；
Appended drawing reference: 1, reaction tower, 2, reboiler, 3, controller, 4, exhaust outlet, 5, discharge port, 6, circulation port, 7, feed back
Mouthful, 8, first charging aperture, 9, second charging aperture, 10, flowmeter, 11, regulating valve, 12, temperature sensor, 13, pressure sensor,
14, liquidometer, 15, heating agent regulating valve, 16, column plate, 17, packing layer, 18, condenser, 19, gas-guide tube, 20, spray tube, 21, spray
Head.
Specific embodiment
The utility model will be described further by specific embodiment below:
Embodiment 1
Preferred embodiment of the present embodiment as the utility model, it discloses a kind of for the anti-of continuous production organosilicon
Tower is answered, specific structure is as shown in Figure 1, include reaction tower 1, condenser 18, reboiler 2 and controller 3, the reaction tower 1 is pressed
It is disposed with exhaust outlet 4, inlet port and outlet port 5 according to sequence from top to bottom, middle charging aperture includes 8 He of first charging aperture
Second charging aperture 9, the first charging aperture 8 and second charging aperture 9 are set in the same level of reaction tower 1, and first into
Angle between 9 axis of material mouth 8 and second charging aperture is 0 ° -180 °；It is also set in the first charging aperture 8 and second charging aperture 9
Be equipped with flowmeter 10 and regulating valve 11, the flowmeter 10 and regulating valve 11 respectively with the input terminal of controller 3 and output end phase
Even；The exhaust outlet 4 connects condenser 18 by pipeline, and the outlet end of the condenser 18 by pipeline and is set to reaction tower
The feedback outlet 7 on top is connected to, and is additionally provided on condenser 18 for hydrogen chloride gas to be drawn out to down leading for one of production process
Tracheae 19；The bottom of the reaction tower 1 is additionally provided with feedback outlet 7, discharge port 5 and circulation port 6, wherein discharge port 5 and circulation port 6
Be connected after being connected with each other by threeway with the bottom of reaction tower 1, the feedback outlet 7 and circulation port 6 by pipeline respectively with boil again
The outlet end of device 2 is connected with input end, and the reboiler 2 is Steam reboiler or conduction oil reboiler, and its steam inlet end
It is provided with the heating agent regulating valve 15 being connected with controller 3；Spray tube 20 is provided in the reaction tower 1, the spray tube 20 divides
It is not connected to first charging aperture 8 and second charging aperture 9, is provided with spray head 21 on the spray tube 20；It is also set in the reaction tower 1
It is equipped with column plate 16；Temperature sensor 12 and pressure sensor 13 are provided in the reaction tower 1, temperature sensor 12 and pressure pass
Sensor 13 is connected with the input terminal of controller 3 respectively, is additionally provided in 1 bottom of reaction tower and is connected with 3 input terminal of controller
Liquidometer 14, the output end of controller 3 is separately connected regulating valve 11 and heating agent regulating valve 15；The controller 3 is independently to set
The control computer or the central control room in chemical plant etc. set.
Embodiment 2
Another embodiment of the present embodiment as the utility model, as shown in figure 3, being provided on its reaction tower 1
One feed inlet 8 and second charging aperture 9, the first charging aperture 8 and second charging aperture 9 are set to the different height of reaction tower 1, and
Angle between 9 axis of first charging aperture 8 and second charging aperture is 0 ° -180 °；The circulation port 6 and discharge port 5 are respectively set
In being provided with packing layer 17 in 1 bottom of reaction tower, the reaction tower 1.
Embodiment 3
Another embodiment of the present embodiment as the utility model is provided with 8 He of first charging aperture on reaction tower 1
Second charging aperture 9, the first charging aperture 8 and second charging aperture 9 are connected after intersecting with reaction tower 1.
Working principle of the utility model is: the utility model is divided by first charging aperture and second charging aperture into reaction tower
Be not passed through chlorosilane (its main component be one or more of trichlorosilane, dichlorosilane, silicon tetrachloride) and ethyl alcohol (or
Hydroxy reaction), silicon tetrachloride and ethyl alcohol (or hydroxy reaction) reaction generate esters of silicon acis and hydrogen chloride, due to chlorosilane, second
(wherein silicon tetrachloride is 53 DEG C to the difference of alcohol, hydrogen chloride and esters of silicon acis boiling point, and ethyl alcohol is 78 DEG C, and hydrogen chloride is -85 DEG C, silicic acid
Ester boiling point is higher than 100 DEG C), therefore react the hydrogen chloride generated and entered in condenser in a manner of gaseous by exhaust outlet, lead to
Cross condensation will be chlorinated the chlorosilane liquefaction contained in the gas that hydrogen is taken out of and finally flowing back into continued to participate in tower body it is anti-
It answers, and hydrogen chloride gas is then directed to by gas-guide tube using hydrogen chloride gas as in the production process of unstripped gas；React the silicon generated
Acid esters then enters reaction tower bottom together with chlorosilane and ethyl alcohol (hydroxy reaction) under gravity, and circulation port will react
The material of tower bottom, which exports in reboiler, to be heated, due to the difference of boiling point, at the heating of reboiler
After reason, chlorosilane and ethyl alcohol (hydroxy reaction) gasify, and esters of silicon acis then keeps liquid constant；The esters of silicon acis of liquid from return liquid
Pipe re-enters into reaction tower bottom and is diluted, heats to the material of reaction tower bottom accumulation, to further increase product
Purity；And gaseous chlorosilane and ethyl alcohol (hydroxy reaction) then flow back into and participate in reaction in reaction tower；When reaction tower bottom
Material when being accumulated to a certain amount of controller open the recycling that the regulating valve on discharge port realizes final products.
The recycling of the reaction of reaction tower described in the utility model, exhaust-gas treatment and final products known to above-mentioned narration
It can be carried out continuously, compared with traditional production method, not only substantially increase production efficiency；Reaction in simultaneous reactions tower
Product all-the-time stable is in a lower level, and then all-the-time stable is in a higher level for reactant, therefore it is conducive to
Reaction is promoted to move towards the direction for generating final products, so that the utilization rate of reaction speed and raw material is substantially increased, and due to
The utility model is able to carry out continuous production, therefore hydrogen chloride gas of its production not only measures larger, and stable yield, therefore this
Utility model can link with by the Chemical Manufacture of raw material of hydrogen chloride gas, with traditional dissolution process and neutralisation treatment
It compares, not only greatly reduces environment protection emission, and substantially increase the economic benefit of enterprise, therefore is described in the utility model anti-
Answer tower economic value with higher and practical value.
Claims (8)
1. a kind of reaction tower for continuous production organosilicon, including reaction tower (1), reboiler (2) and controller (3), special
Sign is: being disposed with exhaust outlet (4), inlet port and outlet port (5) under upper on the reaction tower (1)；The reaction
Be additionally provided with circulation port (6) and feedback outlet (7) on tower (1), the outlet end of the reboiler (2) and input end respectively with circulation port
(6) it is connected with feedback outlet (7).
2. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the feed inlet
Including first charging aperture (8) and second charging aperture (9), stream is provided in the first charging aperture (8) and second charging aperture (9)
Meter (10) and regulating valve (11), the flowmeter (10) and regulating valve (11) be connected respectively with controller (3).
3. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the reaction tower
(1) temperature sensor (12) and pressure sensor (13) being connected with controller (3) are additionally provided in.
4. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the reaction tower
(1) bottom is provided with liquidometer (14), is provided on discharge port (5) regulating valve (11), the liquidometer (14) and regulating valve
(11) it is connected respectively with controller (3).
5. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the reboiler
(2) it is Steam reboiler or conduction oil reboiler, is provided with the heating agent tune being connected with controller (3) on the entrance of reboiler (2)
It saves valve (15).
6. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the reaction tower
(1) multiple column plates (16) or packing layer (17) are additionally provided in.
7. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the exhaust outlet
(4) it is connected with condenser (18), the feedback outlet (7) being connected with reaction tower (1) is provided on the condenser (18) and is used on
The gas-guide tube (19) of tail gas is discharged.
8. a kind of reaction tower for continuous production organosilicon according to claim 1, it is characterised in that: the reaction tower
(1) it is additionally provided with the spray tube (20) being connected with feed inlet in, is provided with spray head (21) on the spray tube (20).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821652930.5U CN209093380U (en) | 2018-10-12 | 2018-10-12 | A kind of reaction tower for continuous production organosilicon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821652930.5U CN209093380U (en) | 2018-10-12 | 2018-10-12 | A kind of reaction tower for continuous production organosilicon |
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| CN209093380U true CN209093380U (en) | 2019-07-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111252771A (en) * | 2020-02-26 | 2020-06-09 | 江苏鑫华半导体材料科技有限公司 | Method and system for purifying trichlorosilane |
| CN112657427A (en) * | 2020-12-21 | 2021-04-16 | 内蒙古兴洋科技有限公司 | Control system and method for accurate silane discharging |
-
2018
- 2018-10-12 CN CN201821652930.5U patent/CN209093380U/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111252771A (en) * | 2020-02-26 | 2020-06-09 | 江苏鑫华半导体材料科技有限公司 | Method and system for purifying trichlorosilane |
| CN111252771B (en) * | 2020-02-26 | 2023-04-07 | 江苏鑫华半导体科技股份有限公司 | Method and system for purifying trichlorosilane |
| CN112657427A (en) * | 2020-12-21 | 2021-04-16 | 内蒙古兴洋科技有限公司 | Control system and method for accurate silane discharging |
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