CN201760276U - Halogenated silane and reaction medium mixing reaction device - Google Patents
Halogenated silane and reaction medium mixing reaction device Download PDFInfo
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- CN201760276U CN201760276U CN201020502746XU CN201020502746U CN201760276U CN 201760276 U CN201760276 U CN 201760276U CN 201020502746X U CN201020502746X U CN 201020502746XU CN 201020502746 U CN201020502746 U CN 201020502746U CN 201760276 U CN201760276 U CN 201760276U
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Abstract
The utility model discloses a halogenated silane and reaction medium mixing reaction device which can enable halogenated silane and reaction medium to be fully contacted and enhance complete reaction so as to improve the quality of reaction products. The reaction device comprises a ring path formed by connection of an inlet and an outlet of a forced circulating device by a connecting pipeline; the ring path is provided with a halogenated silane supplying port, a reaction medium supplying port and a ring path outlet; the ring path outlet is arranged behind the outlet of the forced circulating device; the reaction medium supplying port is arranged before the inlet of the forced circulating device; the halogenated silane and the reaction medium are mixed at the halogenated silane ring path inlet; the halogenated silane ring path inlet is arranged on a connecting pipeline between the reaction medium supplying port and the forced circulating device or the inlet of the forced circulating device; and a dispersing device is further arranged between the halogenated silane supplying port and the halogenated silane ring path inlet and adopts a liquid-phase distributor or a nozzle and the like. The halogenated silane and reaction medium mixing reaction device is especially suitable for being applied to hydrolysis reaction of the halogenated silane.
Description
Technical field
Feed distribution and mixed structure that the utility model relates to a kind of pipe reaction device improve, and this pipe reaction device belongs to two kinds of liquid phase materials of a kind of abundant mixing and realizes the reactor of its continuous feed.
Background technology
At present, the hydrolysis process of domestic dimethyldichlorosilane generally adopts azeotropic hydrochloric acid continuous hydrolysis process, its technology is: join in proportion in the loop reaction mixed reactor of being made up of pipe-line mixer, forced circulation device, the heat exchanger that cold is provided and connecting pipe with dimethyldichlorosilane and as reaction medium " the HCl mass fraction is 18%～22% azeotropic hydrochloric acid ", hydrolysate passes through physical layering, upper oil phase is through neutralization deacidification, washing desalination or remove alkali, promptly obtains the finished product hydrolysate.
Hydrochloric acid provides the said hydrolyzed reaction required water, and dimethyldichlorosilane as long as contact with water hydrolysis just takes place.The hydrolysis that dimethyldichlorosilane is mentioned in the front is extremely rapid, to such an extent as to two just occurred reaction when contacting in pipe-line mixer.In pipe-line mixer, there be the in shortage of water, thereby cause the dimethyldichlorosilane hydrolysis incomplete.In the polysiloxanes that hydrolysis obtains, there is a spot of end group chlorine, this a part of end group chlorine has caused the difficulty of subsequent treatment, its reason is that the activity of the Cl terminal groups on the long linear polysiloxanes is lower, being difficult to remove extremely by neutralization and limited amount washing, desired chlorine residual volume is the content that has neither part nor lot in the chlorine of hydrolysis in the hydrolysate, and the chlorine remnants that are not effectively addressed will cause dimethyldichlorosilane hydrolysate polysiloxanes generation polycondensation reaction, and the viscosity skew takes place.Therefore, there is the deficiency that hydrolysis is incomplete, product chlorine residual volume is bigger in existing mixed reactor.
Existing halogenated silanes and reaction medium mixed reactor mainly comprise by forced circulation device, the loop that heat exchanger and connecting pipe are formed, described loop is provided with the halogenated silanes supply port, reaction medium supply port and loop outlet, by the halogenated silanes supply port, the reactant that the reaction medium supply port enters circulates by the direction of " forced circulation device-heat exchanger-loop outlet " in loop, halogenated silanes mixes in halogenated silanes loop import department with reaction medium, loop exports on the connecting pipe that is arranged between reaction medium supply port and the heat exchanger, heat exchanger is used to control reaction temperature, under the forced circulation device effect, the reactant and the product that enter system flow in order, and are flowed out by the loop outlet.
In existing halogenated silanes and the reaction medium mixed reactor, halogenated silanes has plenty of and directly enters in the loop, have plenty of before entering system, utilize static mixer with halogenated silanes with enter loop after reaction medium mixes, but in known technology for hydrolyzing, mainly be mixing and the reaction that realizes liquid liquid two-phase by aforesaid pipe-line mixer, that is: with halogenated silanes with enter in the loop after reaction medium mixes by pipe-line mixer, it is the halogenated silanes supply port, the reaction medium supply port all is arranged on the pipe-line mixer, the mixing point of halogenated silanes and reaction medium, or be referred to as " import of halogenated silanes loop ", also be at the pipe-line mixer place, its defective is exactly that hydrolysis is incomplete, product chlorine residual volume is bigger.
The connecting pipe of using in the mixed reactor is generally acidproof pipeline.
The utility model content
In order to overcome the deficiency that existing mixed reactor halogenated silanes hydrolysis is incomplete, product chlorine residual volume is bigger, technical problem to be solved in the utility model provides a kind of halogenated silanes that makes and fully contacts with reaction medium, promote complete hydrolysis, thereby improve the halogenated silanes and the reaction medium mixed reactor of hydrolysate quality.
The technical scheme that its technical problem that solves the utility model adopts is: halogenated silanes and reaction medium mixed reactor, comprise the loop that connects to form through connecting pipe by the import of forced circulation device and outlet, described loop is provided with the halogenated silanes supply port, reaction medium supply port and loop outlet, the loop outlet is after the outlet of forced circulation device, the reaction medium supply port is arranged on before the import of forced circulation device, halogenated silanes mixes in halogenated silanes loop import department with reaction medium, the import of described halogenated silanes loop is arranged on the connecting pipe between reaction medium supply port and the forced circulation device or the import department of forced circulation device, also is provided with dispersal device between described halogenated silanes supply port and the import of halogenated silanes loop.
Described forced circulation device is a pump, and the import of described halogenated silanes loop is arranged in its pump chamber.
Described dispersal device is a liquid phase distributor.
Described dispersal device is a shower nozzle.
Be provided with heat exchanger in the described loop, described heat exchanger is arranged between the outlet and loop outlet of forced circulation device.
Be provided with pipe-line mixer between the import of described forced circulation device and the loop outlet, the reaction medium supply port of loop is arranged on the pipe-line mixer.
The beneficial effects of the utility model are: by optimizing the layout of halogenated silanes supply port on the mixed reactor loop, reaction medium supply port and loop outlet, change the feed entrance point and the feeding manner of halogenated silanes in the hydrolytic process, halogenated silanes is fully contacted with reaction medium, promote complete hydrolysis, when reducing hydrolysate viscosity, reduce the halogen residual volume of hydrolysate, saved production cost.
Description of drawings
Fig. 1 is the schematic diagram of existing mixed reactor.
Fig. 2 is the schematic diagram of the utility model mixed reactor.
Fig. 3 is the schematic diagram of another embodiment of the utility model mixed reactor.
Fig. 4 is the schematic diagram of the another embodiment of the utility model mixed reactor.
Fig. 5 is the schematic diagram of a position of halogenated silanes loop import.
Fig. 6 is the schematic diagram of another position of halogenated silanes loop import.
Be labeled as 1-pipe-line mixer, 2-forced circulation device, 3-heat exchanger, 4-dispersal device among the figure, the 5-connecting pipe, the import of 6-halogenated silanes loop, 7-pump chamber, 11-halogenated silanes supply port, 12-reaction medium supply port, the outlet of 13-loop, 20-import, 21-outlet.
The specific embodiment
Below in conjunction with accompanying drawing, embodiment and experiment the utility model is further specified.
Figure 1 shows that existing mixed reactor, it comprises by pipe-line mixer 1, forced circulation device 2, the heat exchanger 3 of cold is provided and connects the loop that connecting pipe 5 is therebetween formed, pipe-line mixer 1 is provided with halogenated silanes supply port 11 and reaction medium supply port 12, enter and hydrolysis takes place immediately and generate hydrolysate after the halogenated silanes of pipe-line mixer 1 and reaction medium mix, under forced circulation device 2 effects, in loop, circulate, and heating under heat exchanger 3 effect, hydrolysate goes to next chemical unit and handles through being arranged on loop outlet 13 on the connecting pipe 5 between pipe-line mixer 1 and the heat exchanger 3.
As Fig. 2, Fig. 3 and shown in Figure 4, halogenated silanes of the present utility model and reaction medium mixed reactor comprise the loop that is connected to form through connecting pipe 5 by the import 20 of forced circulation device 2 and outlet 21, described loop is provided with halogenated silanes supply port 11, reaction medium supply port 12 and loop outlet 13, loop outlet 13 is after the outlet 21 of forced circulation device 2, reaction medium supply port 12 is arranged on before the import 20 of forced circulation device 2, halogenated silanes mixes at halogenated silanes loop import 6 places with reaction medium, described halogenated silanes loop import 6 is arranged on the connecting pipe 5 between reaction medium supply port 12 and the forced circulation device 2 or import 20 places of forced circulation device 2, also is provided with dispersal device 4 between described halogenated silanes supply port 11 and halogenated silanes loop import 6.By changing the feed entrance point and the feeding manner of halogenated silanes in the hydrolytic process, enter the turbulent region that the forced circulation because of reaction medium forms behind the utilization dispersal device 4 refinement halogenated silanes drops again, the mixing fully that has promoted halogenated silanes and reaction medium with fully contact, the quality transmission speed of hydrolytic process is fast, disperse and good mixing effect, the acceleration that is exceedingly fast the hydrolysis process, in the extremely short time of staying, hydrolysate viscosity is lower, reduces the halogen residual volume of hydrolysate simultaneously.
During better scheme is, described forced circulation device 2 is a pump, described loop import 6 is arranged in its pump chamber 7, halogenated silanes after promptly distributing directly enters in the pump chamber 7, then halogenated silanes is after preliminary the dispersion, in pump chamber 7, carry out initial reaction with reaction medium, mixing two-phase that is exceedingly fast and broken two-phase droplet, thus reach the effect of mixing and improving reaction.
Described dispersal device 4 can adopt the chemical industry liquid phase distributor of known conventional, as deflection plate etc.
Described dispersal device 4 is preferably shower nozzle, and dispersion effect is better.
Usually, should be provided with heat exchanger 3 in described loop, described heat exchanger 3 is arranged between the outlet 21 and loop outlet 13 of forced circulation device 2, so that the control reaction temperature.
If improve on former pipe-line mixer formula reaction unit basis, described pipe-line mixer 1 operated by rotary motion is between the import 20 and loop outlet 13 of forced circulation device 2, and the reaction medium supply port 12 that still can keep loop is on pipe-line mixer 1.
Halogenated silanes of the present utility model and reaction medium mixed reactor halogenated silanes applicatory can be dimethyldichlorosilane, monomethyl dichlorosilane, trim,ethylchlorosilane, diphenyl dichlorosilane etc., and reaction medium can be aqueous hydrochloric acid solution, methanol aqueous solution, aqueous sodium carbonate, sodium-chloride water solution of water, variable concentrations etc.
Embodiment one:
As Fig. 2 and shown in Figure 5, halogenated silanes of the present utility model and reaction medium mixed reactor comprise the loop that is connected to form through connecting pipe 5 by the import 20 of forced circulation device 2 and outlet 21, described loop is provided with halogenated silanes supply port 11, reaction medium supply port 12 and loop outlet 13, loop outlet 13 is after the outlet 21 of forced circulation device 2, reaction medium supply port 12 is arranged on before the import 20 of forced circulation device 2, halogenated silanes mixes at halogenated silanes loop import 6 places with reaction medium, halogenated silanes loop import 6 is arranged on the connecting pipe 5 between the import 20 of reaction medium supply port 12 and forced circulation device 2, also be provided with dispersal device 4 between described halogenated silanes supply port 11 and halogenated silanes loop import 6, product is through forced circulation device 2, heat exchanger 3, loop outlet 13 is flowed out.
Embodiment two:
As shown in Figure 3, halogenated silanes of the present utility model and reaction medium mixed reactor comprise the loop that is connected to form through connecting pipe 5 by the import 20 of forced circulation device 2 and outlet 21, described loop is provided with halogenated silanes supply port 11, reaction medium supply port 12 and loop outlet 13, loop outlet 13 is after the outlet 21 of forced circulation device 2, reaction medium supply port 12 is arranged on before the import 20 of forced circulation device 2, halogenated silanes mixes at halogenated silanes loop import 6 places with reaction medium, halogenated silanes loop import 6 is arranged in the pump chamber 7 as the pump of forced circulation device 2, also is provided with dispersal device 4 between described halogenated silanes supply port 11 and halogenated silanes loop import 6.
Embodiment three:
Present embodiment is formed by the existing mixed reactor transformation that is provided with pipe-line mixer 4.As Fig. 4 and shown in Figure 6, halogenated silanes of the present utility model and reaction medium mixed reactor comprise the loop of being made up of pipe-line mixer 4, forced circulation device 2, heat exchanger 3 and connecting pipe 5, reaction medium supply port 12 still is arranged on the pipe-line mixer 4, and halogenated silanes arrives halogenated silanes loop import 6 places that are arranged on the forced circulation device 2 and mixes with reaction medium through halogenated silanes supply port 11, dispersal device 4.
Experiment one:
Do the contrast experiment with the former mixed reactor of Hydrolyze method process using of dimethyldichlorosilane and azeotropic hydrochloric acid and the mixed reactor of the utility model embodiment one, reaction medium is an azeotropic hydrochloric acid.
Adopt former mixed reactor, respectively with 2m
3/ h and 8m
3The flow of/h enters into the loop system of being made up of pipe-line mixer 1, forced circulation device 2, the heat exchanger 3 that cold is provided and connecting pipe 5 continuously with dimethyldichlorosilane and azeotropic hydrochloric acid, and hydrolysis temperature is controlled at 0 ℃～40 ℃.Hydrolysate is by physical layering, and upper oil phase is through neutralization deacidification, washing desalination or remove alkali, obtains the finished product hydrolysate.
Adopt the mixed reactor of the utility model embodiment one, with 2m
3The dimethyldichlorosilane of/h enters into the connecting pipe 5 between forced circulation device 2 and the pipe-line mixer 1 after distributing as the shower nozzle of dispersal device 4, with azeotropic hydrochloric acid with 8m
3/ h flow enters into pipe-line mixer 1, and hydrolysis temperature is controlled at 0 ℃～40 ℃.Hydrolysate is by physical layering, and upper oil phase is through neutralization deacidification, washing desalination or remove alkali, obtains the finished product hydrolysate.
Two kinds of finished product hydrolysate analysis result such as following tables one that device produces.
Table one
| Reaction unit | Acid content (ppm) | Viscosity (mPas) |
| Former mixed reactor | 316 | 12.44 |
| Mixed reactor of the present utility model | 7.02 | 6.35 |
When adopting mixed reactor of the present utility model, the hydrolysate acid content can be controlled at below the 10ppm.This hydrolysate can be used for synthetic 107 glue, cracking and the ring body rectifying two procedures that so can save original arts demand through simple the processing.
Experiment two:
Do the contrast experiment with the mixed reactor that the former mixed reactor of Hydrolyze method process using and the utility model of monomethyl dichlorosilane and trim,ethylchlorosilane pre-composition and water are executed example three, reaction medium is a water.
Adopt former mixed reactor, behind monomethyl dichlorosilane and trim,ethylchlorosilane premix, pre-composition and water directly enter in the reaction unit by the flow of 100L/h and 1000L/h respectively, 0 ℃～40 ℃ of control hydrolysis temperatures.Hydrolysate is through physical separation, and oil phase obtains containing hydrogen silicone oil through neutralization after the filtration.The containing hydrogen silicone oil analysis result sees the following form two.
Adopt the mixed reactor of the utility model embodiment three, behind monomethyl dichlorosilane and trim,ethylchlorosilane premix, pre-composition enters into the pump chamber 7 of the forced circulation pump of loop by 100L/h after shower nozzle distributes, water enters in the reaction unit by the flow of 1000L/h, 0 ℃～40 ℃ of control hydrolysis temperatures.Hydrolysate is through physical separation, and oil phase obtains containing hydrogen silicone oil through neutralization after the filtration.The containing hydrogen silicone oil analysis result sees the following form two.
| Reaction unit | Acid content (ppm) | Hydrogen content (%) |
| Former mixed reactor | 303 | 1.39 |
| Mixed reactor of the |
11 | 1.58 |
Claims (6)
1. halogenated silanes and reaction medium mixed reactor, comprise the loop that connects to form through connecting pipe (5) by the import (20) of forced circulation device (2) and outlet (21), described loop is provided with halogenated silanes supply port (11), reaction medium supply port (12) and loop outlet (13), loop outlet (13) is after the outlet (21) of forced circulation device (2), the import (20) that reaction medium supply port (12) is arranged on forced circulation device (2) before, halogenated silanes is located to mix in halogenated silanes loop import (6) with reaction medium, it is characterized in that: connecting pipe (5) import (20) last or forced circulation device (2) that described halogenated silanes loop import (6) is arranged between reaction medium supply port (12) and the forced circulation device (2) is located, and also is provided with dispersal device (4) between described halogenated silanes supply port (11) and halogenated silanes loop import (6).
2. halogenated silanes as claimed in claim 1 and reaction medium mixed reactor is characterized in that: described forced circulation device (2) is a pump, and described halogenated silanes loop import (6) is arranged in its pump chamber (7).
3. halogenated silanes as claimed in claim 1 or 2 and reaction medium mixed reactor is characterized in that: described dispersal device (4) is a liquid phase distributor.
4. halogenated silanes as claimed in claim 1 or 2 and reaction medium mixed reactor is characterized in that: described dispersal device (4) is a shower nozzle.
5. halogenated silanes as claimed in claim 1 or 2 and reaction medium mixed reactor is characterized in that: be provided with heat exchanger (3) in the described loop, described heat exchanger (3) is arranged between the outlet (21) and loop outlet (13) of forced circulation device (2).
6. halogenated silanes as claimed in claim 5 and reaction medium mixed reactor, it is characterized in that: be provided with pipe-line mixer (1) between the import (20) of described forced circulation device (2) and the loop outlet (13), the reaction medium supply port (12) of loop is arranged on the pipe-line mixer (1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201020502746XU CN201760276U (en) | 2010-08-24 | 2010-08-24 | Halogenated silane and reaction medium mixing reaction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201020502746XU CN201760276U (en) | 2010-08-24 | 2010-08-24 | Halogenated silane and reaction medium mixing reaction device |
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| Publication Number | Publication Date |
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| CN201760276U true CN201760276U (en) | 2011-03-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201020502746XU Expired - Lifetime CN201760276U (en) | 2010-08-24 | 2010-08-24 | Halogenated silane and reaction medium mixing reaction device |
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| CN (1) | CN201760276U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003477A (en) * | 2019-05-20 | 2019-07-12 | 张巧枝 | A kind of polydimethylsiloxane safe production equipment |
-
2010
- 2010-08-24 CN CN201020502746XU patent/CN201760276U/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110003477A (en) * | 2019-05-20 | 2019-07-12 | 张巧枝 | A kind of polydimethylsiloxane safe production equipment |
| CN110003477B (en) * | 2019-05-20 | 2021-09-14 | 胡海明 | Safe production equipment for polydimethylsiloxane |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20110316 Effective date of abandoning: 20120502 |