CN109485669A - A kind of production line and its production method of folded tower method production trim,ethylchlorosilane - Google Patents
A kind of production line and its production method of folded tower method production trim,ethylchlorosilane Download PDFInfo
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- CN109485669A CN109485669A CN201811402192.3A CN201811402192A CN109485669A CN 109485669 A CN109485669 A CN 109485669A CN 201811402192 A CN201811402192 A CN 201811402192A CN 109485669 A CN109485669 A CN 109485669A
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- Prior art keywords
- pipe
- hydrogen chloride
- tower
- chloride gas
- side wall
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 85
- 238000000034 method Methods 0.000 title claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 103
- 239000007789 gas Substances 0.000 claims abstract description 93
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 93
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 93
- 238000006243 chemical reaction Methods 0.000 claims abstract description 79
- 238000010438 heat treatment Methods 0.000 claims abstract description 61
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims abstract description 56
- 230000000694 effects Effects 0.000 claims abstract description 15
- 239000000284 extract Substances 0.000 claims abstract description 8
- 239000007921 spray Substances 0.000 claims description 68
- 230000000712 assembly Effects 0.000 claims description 36
- 238000000429 assembly Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 17
- 239000000498 cooling water Substances 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 9
- 238000003860 storage Methods 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 210000003298 dental enamel Anatomy 0.000 claims description 4
- 229920002313 fluoropolymer Polymers 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000003303 reheating Methods 0.000 claims description 4
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical compound [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 3
- 238000000066 reactive distillation Methods 0.000 claims description 3
- 230000002787 reinforcement Effects 0.000 claims description 3
- 230000004044 response Effects 0.000 claims description 3
- -1 siloxanes Chemical class 0.000 claims description 3
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 239000012495 reaction gas Substances 0.000 claims 1
- 238000011049 filling Methods 0.000 abstract description 5
- 238000011084 recovery Methods 0.000 abstract description 4
- 239000000047 product Substances 0.000 description 10
- 239000001257 hydrogen Substances 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 150000002431 hydrogen Chemical class 0.000 description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- UHUUYVZLXJHWDV-UHFFFAOYSA-N trimethyl(methylsilyloxy)silane Chemical compound C[SiH2]O[Si](C)(C)C UHUUYVZLXJHWDV-UHFFFAOYSA-N 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229930186147 Cephalosporin Natural products 0.000 description 1
- 241001640558 Cotoneaster horizontalis Species 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229940124587 cephalosporin Drugs 0.000 description 1
- 150000001780 cephalosporins Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035935 pregnancy Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/12—Organo silicon halides
- C07F7/121—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20
- C07F7/123—Preparation or treatment not provided for in C07F7/14, C07F7/16 or C07F7/20 by reactions involving the formation of Si-halogen linkages
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Silicon Compounds (AREA)
Abstract
The present invention relates to a kind of production lines of folded tower method production trim,ethylchlorosilane, including the stuffing rectification column set gradually from top to bottom, board-like reaction tower and heating kettle, it is connected at the top of filling extract rectification tower bottom and board-like reaction tower, by being connect with board-like reaction tower lower sides communicating pipe at the top of heating kettle, board-like reaction tower external wall of upper portion is equipped with hexamethyldisiloxane inlet pipe, be connected on heating kettle side wall for be passed through dry hydrogen chloride gas into hydrogen chloride gas pipe, filling extract rectification top of tower is connected with condenser by escape pipe, condenser bottom is connect by return pipe with stuffing rectification column upper portion side wall, the discharge nozzle for exporting trim,ethylchlorosilane is provided on condenser side wall, the present invention provides a kind of production cost is low, structure is simple, high production efficiency, it is good to promote reaction effect, recovery utilization rate is high and long service life folds Ta Fasheng Produce the production line and its production method of trim,ethylchlorosilane.
Description
Technical field
The present invention relates to the production lines and its production method of a kind of folded tower method production trim,ethylchlorosilane.
Background technique
Trim,ethylchlorosilane is important protection sillylation reagent, is widely used in fragrance and organic drug synthesis
In, with the development of cephalosporins medicine in recent years, making it, demand is also increasing, a large amount of every year using more and more extensive
With meet demand, trim,ethylchlorosilane is mainly converted by hexamethyldisiloxane and is obtained for import, production method mainly have with
Under it is several: 1, SOCL2 method reacts hexamethyldisiloxane with SOCL2, and this method generates by-product SO2, and SOCL2 is used
Amount is very big, is not easy to industrially use；2, dense H2SO4+ ammonium chloride method, the hydrogen chloride and two silicon oxygen of hexamethyl which generates
Alkane reaction, the water of generation are absorbed by the concentrated sulfuric acid, and quantity of three wastes is big, high production cost, it is also difficult to be applied to industrial production；3,PCL5
The by-product of method, reaction is POCL3, can preferably meet industrial production, but the technique is to the purity of hexamethyldisiloxane
More demanding (98% or more content)；4, ALCL3 method, the method yield is lower (77%), and purity is low, and quantity of three wastes is big, and industry is raw
Production is not easy to use；5, hydrogen chloride, but this method is applied to production and there is very big difficulty, or requires at -20 degrees Celsius
It reacts below, or pressurization 1.47Mpa or more reacts, production equipment is more demanding, existing production trim,ethylchlorosilane
Production method high production cost, production equipment take up a large area, and investment is high, react to the more demanding of production, each connection
Conveying equipment required precision between component is larger, meanwhile, the service life of each conveying equipment is big due to the corrosivity of product
It is big to reduce, meanwhile, production efficiency is lower, cannot adequately recycle to the substance after reaction, consumed resource is larger, is used for
The reaction tower rush reaction efficiency of reaction is low, is not able to satisfy increasing yield requirement, it is limited to promote reaction effect.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide, a kind of production cost is low, structure is simple, raw
Produce it is high-efficient, promote that reaction effect is good, recovery utilization rate is high and long service life folds the production line of tower method production trim,ethylchlorosilane
And its production method.
The technical scheme of the present invention is realized as follows: a kind of production line of folded tower method production trim,ethylchlorosilane, special
Sign is: including the stuffing rectification column (1), board-like reaction tower (2) and heating kettle (3) set gradually from top to bottom, the filler
It is connected at the top of rectifying column (1) bottom and board-like reaction tower (2), is reacted by communicating pipe (4) with board-like at the top of the heating kettle (3)
Tower (2) lower sides connect, and are provided with hexamethyldisiloxane inlet pipe (5) in board-like reaction tower (2) external wall of upper portion, described
Be connected on heating kettle (3) side wall for be passed through dry hydrogen chloride gas into hydrogen chloride gas pipe (6), the stuffing rectification column
(1) top is connected with condenser (8) by escape pipe (7), and condenser (8) bottom passes through return pipe (9) and filling extract rectification
Tower (1) upper portion side wall connects, and the discharge nozzle (10) for exporting trim,ethylchlorosilane is provided on condenser (8) side wall,
Board-like reaction tower (2) bottom is by outlet pipe (21) and heating kettle (3) far from the side side wall into hydrogen chloride gas pipe (6)
Connection, heating kettle (3) bottom is provided with the outlet tube (22) for exporting dilute hydrochloric acid.
Preferentially are as follows: condenser (8) outer cover is equipped with cooler bin (11), connects on the side wall of cooler bin (11) side
There are the circulating water inlet (12) for being passed through cooling water, side side of the cooler bin (11) far from circulating water inlet (12)
The recirculated water return pipe (13) for exporting the cooling water after exchanging heat is connected on wall.
Preferentially are as follows: the muffler (14) for exporting remaining hydrogen chloride gas is connected at the top of the condenser (8), it is described
The one end of muffler (14) far from condenser (8) is connected to after cooler bin (11) side wall with into hydrogen chloride gas pipe (6), described
Blower (15) are provided on muffler (13).
Preferentially are as follows: described into being provided with hydrogen chloride breather valve (16) on hydrogen chloride gas pipe (6).
Preferentially are as follows: the board-like reaction tower (2) includes the tower body (100) in vertical cylinder, and the communicating pipe (4) is separate
One end of heating kettle (3) is connect with tower body (100) lower sides, and the tower body (100) is internal and is located at communicating pipe (4) top point
It is not provided with the first spray assemblies and the second spray assemblies, first spray assemblies include first set gradually from top to bottom
Ring pipe (111) and the first filter plate (112), it is circumferentially equally spaced from each other on first annular pipe (111) side wall to sow discord every setting
Have several first spray tubes (113), second spray assemblies include the second ring pipe (121) set gradually from top to bottom and
Second filter plate (122), it is circumferentially equally spaced from each other from being arranged at intervals with several second sprays on the second ring pipe (121) side wall
It manages (123), first filter plate (112) and the second filter plate (122) upper surface, which uniformly stack to be provided with, several is used for detention six
The detention ring assemblies that tetramethyldisiloxane cooperation hydrogen chloride gas is reacted, described hexamethyldisiloxane inlet pipe (5) one end
It is connect respectively with first annular pipe (111) and the second ring pipe (121), the hexamethyldisiloxane inlet pipe (5) is far from tower body
(100) one end is connected with storage hexamethyldisiloxane case (104), is provided with spray on the hexamethyldisiloxane inlet pipe (5)
Leaching pump (105), the tower body bottom are provided with reservoir (102), and the reservoir (102) passes through outlet pipe (21) and heating kettle
(3) side wall connects, and is connected to by gas outlet (103) with stuffing rectification column (1) bottom at the top of the tower body (100).
Preferentially are as follows: the detention ring assemblies include several equally spaced from each other from the connection ring for being spaced apart same central axis along longitudinal direction
(131), it is provided with newel (132) on the central axis of several connection rings (131), along week on newel (132) side wall
To and be provided between adjacent connection ring (131) several detention plates (133), adjacent connection ring passes through between (131)
Several detention plates (133) are mutually permanently connected.
Preferentially are as follows: several detention plates (133) along newel (132) it is circumferential it is equally spaced from each other sow discord every setting, adjacent two pieces
It is provided between detention plate (133) and reinforces detention plate (134).
Preferentially are as follows: the one end of several first spray tubes (113) far from first annular pipe (111) is longitudinal towards tower body (100)
Axis line offset, the one end of several second spray tubes (123) far from the second ring pipe (121) is towards tower body (100) longitudinal central axis
Line offset.
Preferentially are as follows: the connection ring (131), newel (132), detention plate (133) and reinforce detention plate (134) material
It is that enamel adds fluoroplastics.
The present invention discloses a kind of productions of the high folded tower method production trim,ethylchlorosilane of low energy consumption, cyclic utilization rate
The production method of line, steps are as follows:
1), raw material is put into: spray pump (105) operates normally, and extracts the six of storage hexamethyldisiloxane case (104) inside
Tetramethyldisiloxane is continually fed into the internal first annular pipe of board-like reaction tower (2) by hexamethyldisiloxane inlet pipe (5)
(111) and in the second ring pipe (121), and from several first spray tubes being separately positioned on first annular pipe (111) side wall
(113) several second spray tubes (123) and on the second ring pipe (121) side wall spray downwards, and spray pump (105) controls pregnancy
200 kgs/hour of base disiloxane flow；
2), reactant is passed through: being opened hydrogen chloride breather valve (16), dry hydrogen chloride gas is from into hydrogen chloride gas pipe
(6) it is passed into heating kettle (3), heating kettle (3) runs and heats to dry hydrogen chloride gas, the chlorination after completing heating
Hydrogen controls dry hydrogen chloride from setting importeding into board-like reaction tower (2) communicating pipe (4) at the top of heating kettle (3)
110 kgs/hour of gas flow；
3), reactive distillation: hexamethyldisiloxane is uniformly sprayed respectively to positioned at the first filter plate 112 and the second filter plate
On the detention ring assemblies of 122 upper surfaces, and filled on several connection rings (131), newel (132) and several detention plates (133)
The hydrogen chloride gas of the detention divided, heat drying rises from board-like reaction tower (2) bottom, and reacts with hexamethyldisiloxane,
Gas, which rises from the gas outlet (103) at the top of board-like reaction tower (2), after reaction enters the internal rectifying of stuffing rectification column (1), instead
The mixed chlorinated hydrogen of the water that should be come out forms dilute hydrochloric acid liquid and falls in reservoir (102), and flow back into and add from outlet pipe (21)
In hot kettle (3), it is set outlet tube (22) export in heating kettle (3) bottom；
4) it, is condensed back: condenser (8) work, and entered by being continually fed into cooling water from circulating water inlet (12)
To in cooler bin (11), cooperation cooler (8) is cooled down, and the cooling water after heat exchange is exported from recirculated water return pipe (13), gas
The hydrogen chloride and trim,ethylchlorosilane of state rise and enter in condenser (8) from escape pipe (7), and trim,ethylchlorosilane finished product exists
From discharge nozzle (10) export on condenser (8) side wall under condensation, partially liq passes through return pipe from condenser (8) bottom
(9) it flows back into the rectifying in stuffing rectification column (1) again and improves purity；
5), circular response: opening blower (15), makes to maintain tiny structure in 0~-0.01Mpa inside muffler (14), will be cold
Remaining hydrogen chloride gas in condenser (8) is withdrawn into from muffler (14) into hydrogen chloride gas pipe (6), and flows back to heating kettle
(3) combination drying hydrogen chloride gas is recycled after reheating in.
By using above-mentioned technical proposal, trim,ethylchlorosilane is produced using folded tower method, the filling extract rectification that will be used to react
Tower (1), board-like reaction tower (2) and heating kettle (3) are set gradually from top to bottom, are on the one hand reduced various for conveying reactant
With the conveying equipment of product, while having simplified production line, production cost is reduced, reduces the land occupation face of production equipment
Product, structure is relatively easy, and on the other hand, dry hydrogen chloride gas is entering in heating kettle (3) after heating, quickly on
It rises in board-like reaction tower (2), with the sufficient haptoreaction of hexamethyldisiloxane in board-like reaction tower (2), improves anti-
The efficiency answered, meanwhile, hexamethyldisiloxane is carried out by the detention ring assemblies being arranged in board-like reaction tower (2) sufficient
Detention, cooperates the spraying effect of the first spray assemblies and the second spray assemblies, and after the dry heat risen from the bottom up
Hydrogen chloride gas carries out uniform haptoreaction, improves the whole efficiency of reaction, surplus in the condenser (8) after completing reaction
Remaining hydrogen chloride gas is withdrawn into from muffler (14) into hydrogen chloride gas pipe (6), and flows back to combination drying chlorine in heating kettle (3)
Change after hydrogen reheats and be recycled, whole resource recycling rate is improved, to further decrease whole life
Cost is produced, the discharge of exhaust gas is reduced, product trim,ethylchlorosilane is further improved by cooler bin (11) cooperation condenser (8)
Precipitation efficiency, improve whole speed of production, meanwhile, the mixed chlorinated hydrogen of water that reaction obtains in the board-like reaction tower (2)
Dilute hydrochloric acid is generated after body, the unified outlet tube (22) by setting in heating kettle (3) bottom exports, the processing of waste water is facilitated,
Low, structure that the present invention provides a kind of production costs is simply, high production efficiency, rush reaction effect is good, recovery utilization rate is high and makes
With the production line and its production method of service life long folded tower method production trim,ethylchlorosilane.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is specific embodiment of the invention structural schematic diagram.
Fig. 2 is board-like reaction tower structural schematic diagram in the specific embodiment of the invention.
Fig. 3 is detention ring assemblies schematic view of the front view in the specific embodiment of the invention.
Fig. 4 is detention ring assemblies schematic top plan view in specific embodiment of the invention structure.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
As Figure 1-Figure 4, the invention discloses a kind of production lines of folded tower method production trim,ethylchlorosilane, in the present invention
In specific embodiment, including the stuffing rectification column 1, board-like reaction tower 2 and heating kettle 3 set gradually from top to bottom, the filler
It is connected at the top of 1 bottom of rectifying column and board-like reaction tower 2, passes through communicating pipe 4 and board-like 2 lower part of reaction tower at the top of the heating kettle 3
Side wall connection, is provided with hexamethyldisiloxane inlet pipe 5 in board-like 2 external wall of upper portion of reaction tower, on 3 side wall of heating kettle
Be connected with for be passed through dry hydrogen chloride gas into hydrogen chloride gas pipe 6, pass through escape pipe 7 at the top of the stuffing rectification column 1
It is connected with condenser 8,8 bottom of condenser is connect by return pipe 9 with 1 upper portion side wall of stuffing rectification column, the condenser 8
Be provided with the discharge nozzle 10 for exporting trim,ethylchlorosilane on side wall, board-like 2 bottom of reaction tower by outlet pipe 21 with
Heating kettle 3 is connected far from the side side wall into hydrogen chloride gas pipe 6, and 3 bottom of heating kettle is provided with for exporting dilute hydrochloric acid
Outlet tube 22.
By using above-mentioned technical proposal, stuffing rectification column 1, board-like reaction tower 2 and heating kettle 3 are successively set from top to bottom
It sets, is connected at the top of 1 bottom of stuffing rectification column and board-like reaction tower 2, is connected on 3 side wall of heating kettle for being passed through dry hydrogen chloride
Gas into hydrogen chloride gas pipe 6, dry hydrogen chloride gas is added from entering in heating kettle 3 into hydrogen chloride gas pipe 6
Heat, after completing heating, hydrogen chloride gas enters in board-like reaction tower 2 from the communicating pipe 4 being arranged at the top of heating kettle 3, board-like anti-
It answers and is provided with hexamethyldisiloxane inlet pipe 5 in 2 external wall of upper portion of tower, hexamethyldisiloxane is from hexamethyldisiloxane inlet pipe 5
It enters in board-like reaction tower 2, the hydrogen chloride gas of the heating and drying that cooperate board-like 2 bottom of reaction tower to be passed through is in board-like reaction
Haptoreaction in tower 2, gaseous state trim,ethylchlorosilane after reaction and hydrogen chloride gas entered after rising in stuffing rectification column 1 into
Row rectifying, is connected with condenser 8 by escape pipe 7 at the top of stuffing rectification column 1, and the trim,ethylchlorosilane of finished product is being condensed from setting
Discharge nozzle 10 on 8 side wall of device exports, and board-like 2 bottom of reaction tower is provided with outlet pipe 21, outlet pipe 21 and heating kettle 3 are separate
Side side wall into hydrogen chloride gas pipe 6 connects, and the water obtained for exporting reaction, the hydrogen chloride gas of water mixing portion is formed
After dilute hydrochloric acid, from the processing of 22 uniform effluent of outlet tube of 3 bottom of heating kettle, by using above-mentioned technical proposal, production is reduced
The occupied area of cost and equipment, structure is simple, is up and down in fold the transmitting that tower structure improves reactant and product
Efficiency, and then improve whole production efficiency.
In the specific embodiment of the invention, 8 outer cover of condenser is equipped with cooler bin 11, the 11 side side of cooler bin
The circulating water inlet 12 for being passed through cooling water, the side of the cooler bin 11 far from circulating water inlet 12 are connected on wall
The recirculated water return pipe 13 for exporting the cooling water after exchanging heat is connected on side wall.
By using above-mentioned technical proposal, it is arranged cooler bin 11 outside condenser 8, connects on 11 side side wall of cooler bin
It is connected to circulating water inlet 12, cooler bin 11 is far from being connected with recirculated water return pipe on the side side wall of circulating water inlet 12
13, cooling water enters in cooler bin 11 from circulating water inlet 12, and is adequately exchanged heat with 8 outer wall of condenser, into one
Step improves the condensation effect of condenser 8, to improve the precipitation efficiency of trim,ethylchlorosilane, improves whole production speed
Degree, the cooling water after completing heat exchange are exported from recirculated water return pipe 13.
In the specific embodiment of the invention, it is connected at the top of the condenser 8 for exporting returning for remaining hydrogen chloride gas
Tracheae 14, the one end of the muffler 14 far from condenser 8 are connected to after 11 side wall of cooler bin with into hydrogen chloride gas pipe 6,
Blower 15 is provided on the muffler 13.
By using above-mentioned technical proposal, in order to further reduce the discharge of three industrial wastes, while production cost is reduced
The utilization rate for improving resource, is connected with the muffler 14 for exporting remaining hydrogen chloride gas, muffler 14 at the top of condenser 8
One end far from condenser 8 is connected to after 11 side wall of cooler bin with into hydrogen chloride gas pipe 6, is provided with blower on muffler 13
15, after blower 15 is run, the negative pressure inside muffler 13 is maintained, continues the remaining hydrogen chloride gas of abstraction reaction, from condenser 8
Top is withdrawn into hydrogen chloride gas pipe 6, is cooperated the dry hydrogen chloride gas being passed through to come back in heating kettle 3 and is added
Heat, in order to reaction later, circulating utilization reduces the discharge of the three wastes, while reducing being passed through for hydrogen chloride gas
Amount, the utilization rate for improving resource reduce production cost and energy consumption.
It is described into being provided with hydrogen chloride breather valve 16 on hydrogen chloride gas pipe 6 in the specific embodiment of the invention.
By using above-mentioned technical proposal, the intake of dry hydrogen chloride gas is controlled for convenience, matches it
The input amount for closing hexamethyldisiloxane is reacted, to promote the reactant of reaction can be balanced, into hydrogen chloride gas pipe 6
On be provided with hydrogen chloride breather valve 16.
In the specific embodiment of the invention, the board-like reaction tower 2 includes the tower body 100 in vertical cylinder, the company
The one end of siphunculus 4 far from heating kettle 3 is connect with 100 lower sides of tower body, inside the tower body 100 and is located at 4 top of communicating pipe
The first spray assemblies and the second spray assemblies are respectively arranged with, first spray assemblies include set gradually from top to bottom
One ring pipe 111 and the first filter plate 112, if circumferentially equally spaced from each other from being arranged at intervals on 111 side wall of first annular pipe
Dry first spray tube 113, second spray assemblies include the second ring pipe 121 and the second filter plate set gradually from top to bottom
122, it is circumferentially equally spaced from each other from being arranged at intervals with several second spray tubes 123 on 121 side wall of the second ring pipe, described
One filter plate 112 and 122 upper surface of the second filter plate uniformly stack be provided with it is several for detention hexamethyldisiloxane cooperate chlorine
Change the detention ring assemblies that are reacted of hydrogen, described 5 one end of hexamethyldisiloxane inlet pipe respectively with first annular pipe 111 and
The connection of second ring pipe 121, the hexamethyldisiloxane inlet pipe 5 are connected with storage two silicon of hexamethyl far from one end of tower body 100
Oxygen alkane case 104 is provided with spray pump 105 on the hexamethyldisiloxane inlet pipe 5, and the tower body bottom is provided with reservoir
102, the reservoir 102 connect by outlet pipe 21 with 3 side wall of heating kettle, pass through at the top of the tower body 100 gas outlet 103 and
The connection of 1 bottom of stuffing rectification column.
By using above-mentioned technical proposal, it is connected with communicating pipe 4 on spray 100 lower sides of tower body, is heated and dry
Hydrogen chloride gas from enter communicating pipe 4 spray tower body 100 inside, spray 100 side of tower body be provided with storage hexamethyl two
Siloxanes case 104 stores up and is provided with spray pump 105 above hexamethyldisiloxane case 104, under the extraction effect of spray pump 105,
The raw material hexamethyldisiloxane inside storage hexamethyldisiloxane case 104 is persistently extracted by hexamethyldisiloxane inlet pipe 5,
And each lead into first annular pipe 111 and the second ring pipe 121, it is circumferentially equally spaced from each other on first annular 111 side wall of pipe
From being arranged at intervals with several first spray tubes 113, if circumferentially equally spaced from each other from being arranged at intervals on 121 side wall of the second ring pipe
Dry second spray tube 123, by several first spray tubes 113 and several second spray tubes 123 by raw material hexamethyldisiloxane
It is uniformly sprayed on the detention ring assemblies for being located at 122 upper surface of the first filter plate 112 and the second filter plate respectively, detention ring assemblies are equal
Even stacking is arranged in 122 upper surface of the first filter plate 112 and the second filter plate, is adequately hindering the detention of raw material hexamethyldisiloxane
It stays on ring assemblies, improves the utilization rate of raw material, the feed throughput in the unit time greatly promotes, for cooperating the chlorine risen
Change hydrogen to be reacted, the contact surface of hydrogen chloride gas and hexamethyldisiloxane is increased, to improve spray raw material
The effect of hexamethyldisiloxane, meanwhile, accelerate the reaction efficiency of hydrogen chloride gas Yu raw material hexamethyldisiloxane, chlorination
Hydrogen rises and with after raw material hexamethyldisiloxane haptoreaction, and obtained trim,ethylchlorosilane rises and passes through gas outlet
103 export.
In the specific embodiment of the invention, the detention ring assemblies include several equally spaced from each other same from being spaced apart along longitudinal direction
The connection ring 131 of central axis is provided with newel 132,132 side wall of newel on the central axis of several connection rings 131
On several detention plates 133 are provided with circumferentially and between adjacent connection ring 131, pass through between adjacent connection ring 131
Several detention plates 133 are mutually permanently connected.
By using above-mentioned technical proposal, to persistently spray raw material in the first spray assemblies and the second spray assemblies spray
After in hexamethyldisiloxane to detention ring assemblies, raw material hexamethyldisiloxane is in several connection rings 131 and detention plate 133
On adequately by detention, hydrogen chloride gas be evenly distributed in after rising several longitudinal directions it is equally spaced from each other sow discord every connection ring 131
Between several detention plates 133, above structure improves the distribution of gas-liquid, takes full advantage of 131 surface of connection ring and detention plate
133 surfaces make raw material hexamethyldisiloxane and the full and uniform haptoreaction of hydrogen chloride gas, and treating capacity is compared with the prior art
50 or more percent is promoted, the reacting dose of processing raw material greatly promotes in the unit time, improves the efficiency and spray of spray
Effect, and improve the purity Coriolis mass for the finished product trim,ethylchlorosilane that reaction obtains.
In the specific embodiment of the invention, several detention plates 133 along newel 132 it is circumferential it is equally spaced from each other sow discord every setting,
It is provided between adjacent two pieces of detention plate 133 and reinforces detention plate 134.
By using above-mentioned technical proposal, several detention plates 133 equally spaced from each other are sowed discord every setting along newel 132 is circumferential
It sets, makes to spray the raw material hexamethyldisiloxane on detention plate 133 and several connection rings 131 and be evenly distributed in detention ring group
On part, is uniformly adequately reacted with the hydrogen chloride gas progress to come up is risen, improve reaction efficiency and effect.In order to further mention
Height promotees reaction efficiency and improves raw material availability, adjacent two to the detention effect of raw material hexamethyldisiloxane to improve
It is provided between the detention plate 133 of block and reinforces detention plate 134, while improving the structural strength of detention board group part entirety, improved
Service life.
In the specific embodiment of the invention, the one end of several first spray tubes 113 far from first annular pipe 111 is towards tower body
100 longitudinal central axis line offsets, the one end of several second spray tubes 123 far from the second ring pipe 121 is towards 100 longitudinal central axis of tower body
Line offset.
By using above-mentioned technical proposal, in order to further increase the spray effect of the first spray assemblies and the second spray assemblies
Fruit guarantees spray in place, and one end by several first spray tubes 113 far from first annular pipe 111 is longitudinal towards spray tower body 100
Axis line offset, one end direction spray tower body 100 longitudinal central axis line of several second spray tubes 123 far from the second ring pipe 121
Offset.
In the specific embodiment of the invention, the connection ring 131, newel 132, detention plate 133 and reinforcement detention plate 134
Material be that enamel adds fluoroplastics.
Hydrogen chloride gas is prevented by using above-mentioned technical proposal in order to further increase the service life of detention board group part
The material of connection ring 131, newel 132, detention plate 133 and reinforcement detention plate 134 is disposed as enamel and added by the corrosion of body
Fluoroplastics.
The present invention discloses a kind of productions of the high folded tower method production trim,ethylchlorosilane of low energy consumption, cyclic utilization rate
The production method of line, steps are as follows:
1), raw material is put into: spray pump 105 operates normally, and extracts the hexamethyl inside storage hexamethyldisiloxane case 104
Disiloxane is continually fed into the first annular pipe 111 and second inside board-like reaction tower 2 by hexamethyldisiloxane inlet pipe 5
In ring pipe 121, and from several first spray tubes 113 and the second ring pipe being separately positioned on first annular 111 side wall of pipe
Several second spray tubes 123 on 121 side walls spray downwards, and 200 kilograms of hexamethyldisiloxane flow of the control of spray pump 105/
Hour；
2), reactant is passed through: opening hydrogen chloride breather valve 16, dry hydrogen chloride gas leads to from into hydrogen chloride gas pipe 6
Enter into heating kettle 3, heating kettle 3 run simultaneously dry hydrogen chloride gas is heated, complete heating after hydrogen chloride gas from
Importeding into communicating pipe 4 in board-like reaction tower 2 for 3 top of heating kettle is set, it is public to control dry hydrogen chloride gas flow 110
Jin/hour；
3), reactive distillation: hexamethyldisiloxane is uniformly sprayed respectively to positioned at the first filter plate 112 and the second filter plate
On the detention ring assemblies of 122 upper surfaces, and adequately hindered on several connection rings 131, newel 132 and several detention plates 133
It stays, the hydrogen chloride gas of heat drying rises from board-like 2 bottom of reaction tower, and reacts with hexamethyldisiloxane, gas after reaction
Body, which rises from the gas outlet 103 at board-like 2 top of reaction tower, enters 1 inside rectifying of stuffing rectification column, the water mixing reflected
Hydrogen chloride forms dilute hydrochloric acid liquid whereabouts and flow back into heating kettle 3 into reservoir 102, and from outlet pipe 21, is set and is adding
The outlet tube 22 of hot 3 bottom of kettle exports；
4), be condensed back: condenser 8 works, and is entered by being continually fed into cooling water from circulating water inlet 12 cold
But in case 11, cooperation cooler 8 is cooled down, and the cooling water after heat exchange is exported from recirculated water return pipe 13, gaseous hydrogen chloride
Rise with trim,ethylchlorosilane and entered in condenser 8 from escape pipe 7, trim,ethylchlorosilane finished product is under condensation from cold
Discharge nozzle 10 on 8 side wall of condenser exports, and partially liq is flowed back into stuffing rectification column 1 from 8 bottom of condenser by return pipe 9
Again rectifying improves purity；
5), circular response: opening blower 15, makes to maintain tiny structure in 0~-0.01Mpa inside muffler 14, by condenser
Remaining hydrogen chloride gas in 8 is withdrawn into from muffler 14 into hydrogen chloride gas pipe 6, and flows back to combination drying in heating kettle 3
Hydrogen chloride gas is recycled after reheating.
By using above-mentioned technical proposal, trim,ethylchlorosilane is produced using folded tower method, the filling extract rectification that will be used to react
Tower 1, board-like reaction tower 2 and heating kettle 3 are set gradually from top to bottom, are on the one hand reduced various for conveying reactant and generation
The conveying equipment of object while having simplified production line, reduces production cost, reduces the occupied area of production equipment, structure
It is relatively easy, on the other hand, after dry hydrogen chloride gas heats in entering heating kettle 3, quickly rise to board-like
In reaction tower 2, the sufficient haptoreaction of hexamethyldisiloxane with board-like reaction tower 2 improves the efficiency of reaction, together
When, sufficient detention, cooperation first are carried out to hexamethyldisiloxane by the detention ring assemblies being arranged in board-like reaction tower 2
Hydrogen chloride gas after the spraying effect of spray assemblies and the second spray assemblies, and the dry heat that rises from the bottom up carries out
Uniform haptoreaction, improves the whole efficiency of reaction, and the remaining hydrogen chloride gas in condenser 8 after completing reaction is from returning
Tracheae 14 is withdrawn into hydrogen chloride gas pipe 6, and is flowed back to combination drying hydrogen chloride gas in heating kettle 3 and recycled after reheating
It uses, improves whole resource recycling rate, to further decrease whole production cost, reduce the discharge of exhaust gas,
Cooperate condenser 8 to further improve the precipitation efficiency of product trim,ethylchlorosilane by cooler bin 11, improves whole production
Speed, meanwhile, dilute hydrochloric acid is generated after the mixed chlorinated hydrogen of water reacted in board-like reaction tower 2, uniformly passes through setting
Outlet tube 22 in 3 bottom of heating kettle exports, and facilitates the processing of waste water, low, structure that the present invention provides a kind of production costs
Simply, high production efficiency, promote that reaction effect is good, recovery utilization rate is high and long service life folds tower method production trim,ethylchlorosilane
Production line and its production method.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of production line of folded tower method production trim,ethylchlorosilane, it is characterised in that: filled out including what is set gradually from top to bottom
Expect rectifying column (1), board-like reaction tower (2) and heating kettle (3), stuffing rectification column (1) bottom and board-like reaction tower (2) top
Connection, heating kettle (3) top are connect by communicating pipe (4) with board-like reaction tower (2) lower sides, the board-like reaction tower
(2) it is provided with hexamethyldisiloxane inlet pipe (5), is connected on heating kettle (3) side wall dry for being passed through in external wall of upper portion
Dry hydrogen chloride gas into hydrogen chloride gas pipe (6), be connected with condensation by escape pipe (7) at the top of the stuffing rectification column (1)
Device (8), condenser (8) bottom are connect by return pipe (9) with stuffing rectification column (1) upper portion side wall, the condenser (8)
The discharge nozzle (10) for exporting trim,ethylchlorosilane is provided on side wall, board-like reaction tower (2) bottom passes through outlet pipe
(21) it is connect with heating kettle (3) far from the side side wall into hydrogen chloride gas pipe (6), heating kettle (3) the bottom setting is useful
In the outlet tube (22) of export dilute hydrochloric acid.
2. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 1, it is characterised in that: described cold
Condenser (8) outer cover is equipped with cooler bin (11), is connected on the side wall of cooler bin (11) side for being passed through following for cooling water
Ring water water inlet pipe (12), the cooler bin (11) far from circulating water inlet (12) side side wall on be connected with for export change
The recirculated water return pipe (13) of cooling water after heat.
3. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 2, it is characterised in that: described cold
The muffler (14) for exporting remaining hydrogen chloride gas is connected at the top of condenser (8), the muffler (14) is far from condenser
(8) one end is connected to after running through cooler bin (11) side wall with into hydrogen chloride gas pipe (6), is provided with wind on the muffler (13)
Machine (15).
4. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 3, it is characterised in that: it is described into
Hydrogen chloride breather valve (16) are provided on hydrogen chloride gas pipe (6).
5. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 1 or 2 or 3, it is characterised in that:
The board-like reaction tower (2) includes the tower body (100) in vertical cylinder, the one end of the communicating pipe (4) far from heating kettle (3)
It is connect with tower body (100) lower sides, the tower body (100) is internal and is respectively arranged with the first spray above communicating pipe (4)
Drench component and the second spray assemblies, first spray assemblies include the first annular pipe (111) set gradually from top to bottom and
First filter plate (112), it is circumferentially equally spaced from each other from being arranged at intervals with several first sprays on first annular pipe (111) side wall
It manages (113), second spray assemblies include the second ring pipe (121) and the second filter plate (122) set gradually from top to bottom,
It is circumferentially equally spaced from each other from being arranged at intervals with several second spray tubes (123) on second ring pipe (121) side wall, described
One filter plate (112) and the second filter plate (122) upper surface, which uniformly stack to be provided with, several matches for detention hexamethyldisiloxane
Close the detention ring assemblies that are reacted of hydrogen chloride gas, described hexamethyldisiloxane inlet pipe (5) one end respectively with it is first annular
(111) and the second ring pipe (121) connection are managed, the hexamethyldisiloxane inlet pipe (5) connects far from the one end of tower body (100)
There is storage hexamethyldisiloxane case (104), is provided with spray pump (105), the tower on the hexamethyldisiloxane inlet pipe (5)
Body bottom is provided with reservoir (102), and the reservoir (102) is connect by outlet pipe (21) with heating kettle (3) side wall, described
It is connected to by gas outlet (103) with stuffing rectification column (1) bottom at the top of tower body (100).
6. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 5, it is characterised in that: the resistance
It includes several equally spaced from each other from the connection ring (131) for being spaced apart same central axis, several connection rings along longitudinal direction for staying ring assemblies
(131) it is provided on central axis newel (132), circumferentially and positioned at adjacent connection on newel (132) side wall
It is provided with several detention plates (133) between ring (131), it is mutual by several detention plates (133) between adjacent connection ring (131)
It is fixedly connected.
7. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 6, it is characterised in that: several resistances
Stay plate (133) along newel (132) it is circumferential it is equally spaced from each other sow discord every setting, be provided between adjacent two pieces of detention plate (133)
Reinforce detention plate (134).
8. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 5, it is characterised in that: Ruo Gan
It is sprayed towards tower body (100) longitudinal central axis line offset, several second one end of one spray tube (113) far from first annular pipe (111)
The one end of shower pipe (123) far from the second ring pipe (121) is towards tower body (100) longitudinal central axis line offset.
9. a kind of production line of folded tower method production trim,ethylchlorosilane according to claim 7, it is characterised in that: the company
Connecing ring (131), newel (132), detention plate (133) and the material of reinforcement detention plate (134) is that enamel adds fluoroplastics.
10. a kind of production method for the production line for fitting above-mentioned folded tower method production trim,ethylchlorosilane, which is characterized in that step is such as
Under:
1), raw material is put into: spray pump (105) operates normally, and extracts the internal hexamethyl of storage hexamethyldisiloxane case (104)
Disiloxane is continually fed into the internal first annular pipe (111) of board-like reaction tower (2) by hexamethyldisiloxane inlet pipe (5)
In the second ring pipe (121), and from several first spray tubes (113) being separately positioned on first annular pipe (111) side wall
It is sprayed downwards with several second spray tubes (123) on the second ring pipe (121) side wall, spray pump (105) controls hexamethyl two
200 kgs/hour of siloxanes flow；
2), reactant is passed through: being opened hydrogen chloride breather valve (16), dry hydrogen chloride gas leads to from into hydrogen chloride gas pipe (6)
Enter in heating kettle (3), heating kettle (3) runs and heats to dry hydrogen chloride gas, the hydrogen chloride gas after completing heating
Body controls dry hydrogen chloride gas from setting importeding into board-like reaction tower (2) communicating pipe (4) at the top of heating kettle (3)
110 kgs/hour of flow；
3), reactive distillation: hexamethyldisiloxane is uniformly sprayed respectively on the first filter plate 112 and the second filter plate 122
On the detention ring assemblies on surface, and adequately hindered on several connection rings (131), newel (132) and several detention plates (133)
It stays, the hydrogen chloride gas of heat drying rises from board-like reaction tower (2) bottom, and reacts with hexamethyldisiloxane, after reaction
Gas, which rises from the gas outlet (103) at the top of board-like reaction tower (2), enters the internal rectifying of stuffing rectification column (1), reflects
The mixed chlorinated hydrogen of water form dilute hydrochloric acid liquid whereabouts and flow back into heating kettle (3) in reservoir (102), and from outlet pipe (21)
In, it is set outlet tube (22) export in heating kettle (3) bottom；
4) it, is condensed back: condenser (8) work, and entered by being continually fed into cooling water from circulating water inlet (12) cold
But in case (11), cooperation cooler (8) is cooled down, and the cooling water after heat exchange is exported from recirculated water return pipe (13), gaseous
Hydrogen chloride and trim,ethylchlorosilane rise and enter in condenser (8) from escape pipe (7), and trim,ethylchlorosilane finished product is condensing
From discharge nozzle (10) export on condenser (8) side wall under effect, partially liq passes through return pipe (9) from condenser (8) bottom
It flows back into the rectifying in stuffing rectification column (1) again and improves purity；
5), circular response: opening blower (15), makes to maintain tiny structure in 0~-0.01Mpa inside muffler (14), by condenser
(8) the remaining hydrogen chloride gas in is withdrawn into from muffler (14) into hydrogen chloride gas pipe (6), and is flowed back in heating kettle (3)
Combination drying hydrogen chloride gas is recycled after reheating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811402192.3A CN109485669B (en) | 2018-11-22 | 2018-11-22 | Production line for producing trimethylchlorosilane by tower stacking method and production method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811402192.3A CN109485669B (en) | 2018-11-22 | 2018-11-22 | Production line for producing trimethylchlorosilane by tower stacking method and production method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115430393A (en) * | 2022-08-12 | 2022-12-06 | 福建省龙德新能源有限公司 | Reaction tower for producing phosphorus pentafluoride |
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| JPS616833B2 (en) * | 1976-05-24 | 1986-03-01 | Fujisawa Pharmaceutical Co | |
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| JPS616833B2 (en) * | 1976-05-24 | 1986-03-01 | Fujisawa Pharmaceutical Co | |
| CN105367594A (en) * | 2015-10-09 | 2016-03-02 | 浙江硕而博化工有限公司 | Method for preparing hexamethyl-disilazane with hexamethyldisiloxane as raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115430393A (en) * | 2022-08-12 | 2022-12-06 | 福建省龙德新能源有限公司 | Reaction tower for producing phosphorus pentafluoride |
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