CN105777793A - Column-type continuous synthesis method for hexamethyl-disilazane - Google Patents
Column-type continuous synthesis method for hexamethyl-disilazane Download PDFInfo
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- CN105777793A CN105777793A CN201610213931.9A CN201610213931A CN105777793A CN 105777793 A CN105777793 A CN 105777793A CN 201610213931 A CN201610213931 A CN 201610213931A CN 105777793 A CN105777793 A CN 105777793A
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- hexamethyldisiloxane
- ammonia
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- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 title abstract 4
- 238000001308 synthesis method Methods 0.000 title abstract 3
- 238000006243 chemical reaction Methods 0.000 claims abstract description 102
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000007788 liquid Substances 0.000 claims abstract description 45
- 239000000706 filtrate Substances 0.000 claims abstract description 17
- 239000000047 product Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000004570 mortar (masonry) Substances 0.000 claims abstract description 10
- 238000003860 storage Methods 0.000 claims abstract description 5
- 230000004044 response Effects 0.000 claims description 44
- 229910021529 ammonia Inorganic materials 0.000 claims description 33
- 239000007787 solid Substances 0.000 claims description 27
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 19
- 230000002194 synthesizing effect Effects 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 12
- 239000003513 alkali Substances 0.000 claims description 10
- 239000011550 stock solution Substances 0.000 claims description 8
- 238000013517 stratification Methods 0.000 claims description 8
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000010413 mother solution Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 4
- 239000012044 organic layer Substances 0.000 claims description 4
- 208000002925 dental caries Diseases 0.000 claims description 3
- 239000002904 solvent Substances 0.000 abstract description 12
- 230000000903 blocking effect Effects 0.000 abstract description 3
- 238000010790 dilution Methods 0.000 abstract description 3
- 239000012895 dilution Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 abstract 3
- 239000012043 crude product Substances 0.000 abstract 1
- 238000002347 injection Methods 0.000 abstract 1
- 239000007924 injection Substances 0.000 abstract 1
- 230000036632 reaction speed Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000000376 reactant Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000005265 energy consumption Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- GHASVSINZRGABV-UHFFFAOYSA-N Fluorouracil Chemical compound FC1=CNC(=O)NC1=O GHASVSINZRGABV-UHFFFAOYSA-N 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- LKCWBDHBTVXHDL-RMDFUYIESA-N amikacin Chemical compound O([C@@H]1[C@@H](N)C[C@H]([C@@H]([C@H]1O)O[C@@H]1[C@@H]([C@@H](N)[C@H](O)[C@@H](CO)O1)O)NC(=O)[C@@H](O)CCN)[C@H]1O[C@H](CN)[C@@H](O)[C@H](O)[C@H]1O LKCWBDHBTVXHDL-RMDFUYIESA-N 0.000 description 1
- 229960004821 amikacin Drugs 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- UCKZMPLVLCKKMO-LHLIQPBNSA-N cephamycin Chemical compound S1CC(C)=C(C(O)=O)N2C(=O)[C@@H](C)[C@]21OC UCKZMPLVLCKKMO-LHLIQPBNSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 229960002949 fluorouracil Drugs 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 150000002960 penicillins Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 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
- C07F7/10—Compounds having one or more C—Si linkages containing nitrogen having a Si-N linkage
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
Abstract
The invention discloses a column-type continuous synthesis method for hexamethyl-disilazane. According to the column-type continuous synthesis method, first, a storage tank is filled with trimethylsilyl chloride, trimethylsilyl chloride is injected into a first-stage reaction column through a metering pump via a liquid guiding pipe, then ammonia gas is injected directly into the lower portion of the first-stage reaction column through a gas guiding pipe for a reaction, trimethylsilyl chloride is injected from the first-stage reaction column again, the injection speed of ammonia gas is regulated, a material is pumped into an A-stage plate-and-frame filter press to be filtered through a first mortar pump via the liquid guiding pipe, filtrate flows into a second-stage reaction column through the liquid guiding pipe for continuous reaction inside the second-stage reaction column and is pumped into a B-stage plate-and-frame filter press to be filtered through a second mortar pump via the liquid guiding pipe, filtrate which is obtained after being filtered by the B-stage plate-and-frame filter press enters a product receiving groove through the liquid guiding pipe, standing layering is performed on a crude product, and tail gas is recovered. Blocking is avoided, reaction is performed smoothly, and it is avoided that the concentration of the raw material is reduced under dilution of solvent, so that reaction speed is influenced.
Description
Technical field
The present invention relates to a kind of hexamethyldisiloxane pillar method for continuously synthesizing.
Background technology
Hexamethyldisiloxane, molecular formula: C6H19NSi2；[(CH3)2Si]2NH, water white transparency mobile liquid, slightly amine taste, fusing point :-78 DEG C, boiling point: 126.2 DEG C, relative density: 0.7741, refractive index: 1.4078.Trimethyl silanol and hexamethyldisiloxane can be decomposed into rapidly with air contact, be prone to be hydrolyzed into silicon ether and release ammonia under neutrality or weak basic condition, more stable under highly basic, meet acidic materials and vigorous reaction easily occurs.For extraordinary organic synthesis, silylanizing in the building-up processes such as amikacin, penicillin, cephamycin, fluorouracil and various penicillin derivatives, the surface treatment of the powder such as kieselguhr, white carbon, titanium, the adhesive aid etc. of photo-induced etching agent in semi-conductor industry.Can by trim,ethylchlorosilane and NH3Reaction is produced.
On producing during synthesis hexamethyldisiloxane, two molecule trim,ethylchlorosilanes and three molecules of ammonia solid/liquid/gas reactions generate a part hexamethyldisiloxane and two molecule ammonium chloride, and response speed is quickly.Carrying out along with reaction, in reactant liquor, chloride solid gets more and more, reactant liquor is increasingly stuck with paste, stir also more and more difficult, reaction is difficult to continue, often to add substantial amounts of solvent goes dilute reaction solution could maintain being smoothed out of reaction, and the volume adding solvent is 3～4 times of reaction main material trim,ethylchlorosilane volume.Therefore, common production technology is: first add the solvent of 3～4 times of volumes in reactor, add the trim,ethylchlorosilane of 1 times of volume, and stir, starting to pass into ammonia to react, reaction terminates, and pasty state reactant alkali cleaning is layered, water layer centrifugation goes out chloride solid, and organic layer removes rectification separation solvent and product.The addition of a large amount of solvents, makes the concentration of main material significantly dilute, have impact on response speed；Reaction separates and recovers solvent again, has both consumed the energy and also made production efficiency be substantially reduced after terminating.
Summary of the invention
Present invention aim at the deficiency existing for prior art and the technical scheme of a kind of hexamethyldisiloxane pillar method for continuously synthesizing is provided, by two reaction columns and two filter press, effectively the chloride solid produced in reaction is easily separated, avoid clogging, reaction is made to be smoothed out on earth, avoid and because of solvent, the concentration of raw material is diluted, affect response speed, reduce energy consumption.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that
A kind of hexamethyldisiloxane pillar method for continuously synthesizing, it is characterised in that comprise the steps:
1) first trim,ethylchlorosilane is seated in storage tank, open Unidirectional solenoid valve, trim,ethylchlorosilane is squeezed into through liquid conduits toward the top of first order reaction post by dosing pump, trim,ethylchlorosilane is made to be full of first order reaction post, then it is passed directly into ammonia in the bottom of first order reaction post by airway to react, the speed controlling passed into ammonia is 0.1～1.0L/min, ammonia is made to flow from bottom to top, simultaneously close off other valve, the ammonia risen and trim,ethylchlorosilane are fully contacted, and improve reaction rate；
2) question response carries out 20～30min, the bottom chloride solid of first order reaction post gets more and more, material becomes paste gradually, it is that 0.1～0.3L/min squeezes into trim,ethylchlorosilane continuously from the top of first order reaction post by flow again, and regulate ammonia pass into speed to 0.1～0.3L/min, open the outlet of first order reaction column bottom simultaneously, and through liquid conduits material is driven in A level filter press continuously with the first mortar pump and to be filtered, it is maintained with the liquid level of first order reaction post, chloride solid is trapped in A level filter press, filtrate flows into secondary response post through liquid conduits, and control the flow velocity of filtrate；
3) reach after the liquid level set until secondary response post, open and regulate the flow of the passed into ammonia of airway of secondary response post bottom, reaction is continued in secondary response post, the reaction mass making secondary response column outlet place reaches reaction end, and be driven in B level filter press through liquid conduits by the second mortar pump and to be filtered, filtrate after B level sheet frame Filter Press is entered in product receiving slit by liquid conduits, obtains thick product；
4) the thick product (chloride solid) separated regularly is put in alkali liquor, control the concentration of alkali liquor at 5～15mol/L simultaneously, after agitated and stratification, upper organic layer is collected, go to reclaim product, lower floor's material runs out after being centrifuged and reclaims chloride solid, and Recycling Mother Solution uses；
5) reaction end gas produced after first order reaction post and secondary response post react is reclaimed by gas conduit inflow water-jet vacuum pump, recycles after making ammonia.
A large amount of solids owing to producing in first order reaction post are separated timely in A level filter press, ensure that the mobility that reaction mass is good in secondary response post, reaction can be smoothed out on earth, simultaneously because the dilution of non-solubilizer, the concentration of reaction mass is high, response speed is faster, it is effectively shortened the response time, A level, B level filter press are respectively arranged with two, are used alternatingly, it is possible to achieve Total continuity reacts, substantially increase production efficiency, save human resources, owing to not needing recycling design, greatly reduce energy consumption.
Further, step 2) and step 3) in A level filter press and B level filter press all include bracing frame, fixing tailgate, movable plate and locking device, fixing tailgate is fixedly connected on bracing frame, movable plate is positioned at the end of fixing tailgate, and movable plate connects locking device, and locking device is erected on bracing frame, movable plate is under the effect of locking device, screen plate in fixing tailgate is extruded, improves the mobility of stock solution, improve the efficiency of filtration simultaneously.
Further, the both sides up and down of fixing tailgate are provided with water conservancy diversion cavity, the end of the water conservancy diversion cavity being positioned below is provided with stock solution import, the end of water conservancy diversion cavity above is provided with filtrate (liquid, it is evenly arranged with screen plate between two water conservancy diversion cavitys, screen plate is evenly arranged with filtering holes, the two ends up and down of screen plate connect water conservancy diversion cavity respectively through drain pipe and feed tube, the stock solution water conservancy diversion cavity through lower section flows into screen plate uniformly across feed tube, under the effect of filtering holes through drain pipe flow into above water conservancy diversion cavity, final from filtrate (liquid outflow, effectively play the effect filtering chloride solid.
Further, locking device includes handwheel and extrusion spring, and handwheel connects movable plate by extrusion spring, by rotating handwheel, drives movable plate extruding, makes filtering residue discharge filter press.
Further, step 2) in first order reaction post liquid level is first order reaction post height 4/5, this liquid level be possible not only to meet reaction normal need, reactant liquor will not be made to overflow, and it is effectively increased the contact area of ammonia and trim,ethylchlorosilane, improve reaction rate.
Further, step 3) in secondary response post liquid level is secondary response post height 3/4, this liquid level can effectively prevent chloride solid from piling up and cause the blocking of pipeline, and then prevents reactant liquor from overflowing.
Further, step 4) in time of stratification be 5～10min, it is simple to chloride solid separates with mother solution, improves the efficiency reclaimed.
Further, step 4) in alkali liquor be sodium hydroxide solution, sodium hydroxide solution can improve the response rate of reactant liquor.
Further, step 5) in water-jet vacuum pump include condenser pump, check-valves and tail pipe, tail pipe is fixedly connected on the lower section of condenser pump, and check-valves is fixedly connected on the side of condenser pump, and the end of check-valves is provided with vacuum meter, condenser pump can effectively reduce the temperature of reaction end gas, it is easy to reaction end gas is reclaimed, again recycles after making ammonia, it is to avoid contaminated environment, reaction end gas can be detected by vacuum meter, improves safety.
Due to the fact that and have employed technique scheme, have the advantages that
1, a large amount of solids produced in first order reaction post are separated timely in A level filter press, it is ensured that the mobility that reaction mass is good in secondary response post, reaction can be smoothed out on earth；
2, owing to non-solubilizer dilutes, the concentration of reaction mass is high, and response speed faster, is effectively shortened the response time；
3, A level, B level filter press are respectively arranged with two, are used alternatingly, it is possible to achieve Total continuity reacts, and substantially increases production efficiency, has saved human resources, owing to not needing recycling design, greatly reduces energy consumption.
The present invention passes through two reaction columns and two filter press, is effectively easily separated by the chloride solid produced in reaction, it is to avoid result in blockage, reaction is made to be smoothed out on earth, avoid and because of solvent, the concentration of raw material is diluted, affect response speed, reduce energy consumption.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the invention will be further described:
Fig. 1 is the process chart of a kind of hexamethyldisiloxane pillar method for continuously synthesizing of the present invention；
Fig. 2 is the structural representation of A level filter press and B level filter press in the present invention.
In figure: 1-storage tank；2-first order reaction post；3-secondary response post；4-A level filter press；5-B level filter press；6-product receiving slit；7-water-jet vacuum pump；8-dosing pump；9-Unidirectional solenoid valve；10-liquid conduits；11-the first mortar pump；12-airway；13-the second mortar pump；14-gas conduit；15-condenser pump；16-check-valves；17-vacuum meter；18-tail pipe；19-fixes tailgate；20-bracing frame；21-locking device；22-movable plate；23-stock solution import；24-filtrate (liquid；25-screen plate；26-filtering holes；27-drain pipe；28-feed tube；29-handwheel；30-extrusion spring；31-water conservancy diversion cavity.
Detailed description of the invention
As shown in Figure 1 to Figure 2, for one hexamethyldisiloxane pillar method for continuously synthesizing of the present invention, comprise the steps:
1) first trim,ethylchlorosilane is seated in storage tank 1, open Unidirectional solenoid valve 9, trim,ethylchlorosilane is squeezed into through liquid conduits 10 toward the top of first order reaction post 2 by dosing pump 8, trim,ethylchlorosilane is made to be full of first order reaction post 2, then it is passed directly into ammonia in the bottom of first order reaction post 2 by airway 12 to react, controlling the speed of passed into ammonia is 0.1～1.0L/min (ammonia pass into speed the impact of reaction is as shown in table 1), ammonia is made to flow from bottom to top, simultaneously close off other valve, the ammonia risen and trim,ethylchlorosilane are fully contacted, improve reaction rate；
null2) question response carries out 20～30min，The bottom chloride solid of first order reaction post 2 gets more and more，Material becomes paste gradually，It is that 0.1～1.0L/min squeezes into trim,ethylchlorosilane continuously from the top of first order reaction post 2 by flow again，And regulate ammonia pass into speed to 0.1～0.8L/min，Open the outlet bottom first order reaction post 2 simultaneously，And be driven into continuously in A level filter press 4 through 10 materials of liquid conduits with the first mortar pump 11 and to be filtered，It is maintained with the liquid level of first order reaction post 2，The liquid level of first order reaction post 2 is the 4/5 of first order reaction post 2 height，This liquid level is possible not only to meet the normal need of reaction，Reactant liquor will not be made to overflow，And it is effectively increased the contact area of ammonia and trim,ethylchlorosilane，Improve reaction rate，Chloride solid is trapped in A level filter press 4，Filtrate flows into secondary response post 3 through liquid conduits 10，And control the flow velocity of filtrate；
3) reach after the liquid level set until secondary response post 3, open and regulate the passed into ammonia of airway 12 of secondary response post 3 bottom flow (ammonia pass into speed on reaction impact as shown in table 1), reaction is continued in secondary response post 3, the liquid level of secondary response post 3 is the 3/4 of secondary response post 3 height, this liquid level can effectively prevent chloride solid accumulation from causing the blocking of pipeline, and then prevent reactant liquor from overflowing, the reaction mass making secondary response post 3 exit reaches reaction end, and be driven in B level filter press 5 through liquid conduits 10 be filtered by the second mortar pump 13, filtrate after B level filter press 5 filters enters in product receiving slit 6 by liquid conduits 10, obtain thick product；
nullStep 2) and step 3) in A level filter press 4 and B level filter press 5 all include bracing frame 20、Fixing tailgate 19、Movable plate 22 and locking device 21，Fixing tailgate 19 is fixedly connected on bracing frame 20，Movable plate 22 is positioned at the end of fixing tailgate 19，Movable plate 22 connects locking device 21，Locking device 21 is erected on bracing frame 20，Movable plate 22 is under the effect of locking device 21，Screen plate 25 in fixing tailgate 19 is extruded，Improve the mobility of stock solution，Improve the efficiency of filtration simultaneously，The both sides up and down of fixing tailgate 19 are provided with water conservancy diversion cavity 31，The end of the water conservancy diversion cavity 31 being positioned below is provided with stock solution import 23，The end of water conservancy diversion cavity 31 above is provided with filtrate (liquid 24，It is evenly arranged with screen plate 25 between two water conservancy diversion cavitys 31，Screen plate 25 is evenly arranged with filtering holes 26，The two ends up and down of screen plate 25 connect water conservancy diversion cavity 31 respectively through drain pipe 27 and feed tube 28，The stock solution water conservancy diversion cavity 31 through lower section flows into screen plate 25 uniformly across feed tube 28，Under the effect of filtering holes 26 through drain pipe 27 flow into above water conservancy diversion cavity 31，Finally flow out from filtrate (liquid 24，Effectively play the effect filtering chloride solid，Locking device 21 includes handwheel 29 and extrusion spring 30，Handwheel 29 connects movable plate 22 by extrusion spring 30，By rotating handwheel 29，Movable plate 22 is driven to extrude，Filtering residue is made to discharge filter press.
Table 1 ammonia passes into the speed impact on reaction yield
From table 1 it follows that as ammonia speed respectively 0.35L/min and the 0.39L/min passed in first order reaction post 2 and secondary response post 3, reaction yield is up to 95.46%.Course of reaction produces a large amount of indissoluble ground chloride solid, if the ammonia excessive velocities or uneven passed into, it is easily caused reaction can not be smoothed out, affect the final yield of product and quality, if the ammonia speed passed into is excessively slow, the chloride solid crystal grain making generation is relatively big, is unfavorable for the carrying out of reaction.Adopt two reaction columns and two filter press simultaneously, make chloride solid be separated timely, it is possible to be greatly improved the yield of reaction.
4) the thick product (chloride solid) separated regularly is put in alkali liquor, control the concentration of alkali liquor at 5～15mol/L simultaneously, alkali liquor is sodium hydroxide solution, sodium hydroxide solution can improve the response rate of reactant liquor, after agitated and stratification, the time of stratification is 5～10min, it is easy to separating of chloride solid and mother solution, improve the efficiency reclaimed, upper organic layer is collected, going to reclaim product, lower floor's material runs out after being centrifuged and reclaims chloride solid, and Recycling Mother Solution uses；Naoh concentration and stratification time are as described in Table 2 on the impact of reaction yield；
Table 2 naoh concentration and the impact on reaction yield of the stratification time
As shown in Table 2, hexamethyldisiloxane hydrolysis degree in aqueous slkali is less, and along with the increase hydrolysis degree of naoh concentration reduces, after the concentration of sodium hydroxide reaches 8mol/L, hexamethyldisiloxane hydrolysis degree in aqueous slkali varies less.
5) reaction end gas produced after first order reaction post 2 and secondary response post 3 react flows into water-jet vacuum pump 7 by gas conduit 14 and reclaims, recycle after making ammonia, water-jet vacuum pump 7 includes condenser pump 15, check-valves 16 and tail pipe 18, tail pipe 18 is fixedly connected on the lower section of condenser pump 15, check-valves 16 is fixedly connected on the side of condenser pump 15, the end of check-valves 16 is provided with vacuum meter 17, condenser pump 15 can effectively reduce the temperature of reaction end gas, it is easy to reaction end gas is reclaimed, again recycle after making ammonia, avoid contaminated environment, reaction end gas can be detected by vacuum meter 17, improve safety.
A large amount of solids owing to producing in first order reaction post 2 are separated timely in A level filter press 4, ensure that the mobility that reaction mass is good in secondary response post 3, reaction can be smoothed out on earth, simultaneously because the dilution of non-solubilizer, the concentration of reaction mass is high, response speed is faster, it is effectively shortened the response time, A level, B level filter press 5 are respectively arranged with two, are used alternatingly, it is possible to achieve Total continuity reacts, substantially increase production efficiency, save human resources, owing to not needing recycling design, greatly reduce energy consumption.
These are only specific embodiments of the invention, but the technical characteristic of the present invention is not limited thereto.Any based on the present invention, for realizing essentially identical technique effect, done ground simple change, equivalent replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (9)
1. a hexamethyldisiloxane pillar method for continuously synthesizing, it is characterised in that comprise the steps:
1) first trim,ethylchlorosilane is seated in storage tank, open Unidirectional solenoid valve, described trim,ethylchlorosilane is squeezed into through liquid conduits toward the top of first order reaction post by dosing pump, described trim,ethylchlorosilane is made to be full of described first order reaction post, then it is passed directly into ammonia in the bottom of described first order reaction post by airway to react, the speed controlling passed into ammonia is 0.1～1.0L/min, makes ammonia flow from bottom to top, simultaneously closes off other valve；
2) question response carries out 20～30min, it is that 0.1～1.0L/min squeezes into described trim,ethylchlorosilane continuously from the top of described first order reaction post by flow again, and regulate ammonia pass into speed to 0.1～0.8L/min, open the outlet of described first order reaction column bottom simultaneously, and through described liquid conduits material is driven in A level filter press continuously with the first mortar pump and to be filtered, it is maintained with the liquid level of described first order reaction post, chloride solid is trapped in described A level filter press, filtrate flows into secondary response post through described liquid conduits, and control the flow velocity of filtrate；
3) reach after the liquid level set until described secondary response post, open and regulate the flow of the passed into ammonia of airway of described secondary response post bottom, reaction is continued in described secondary response post, the reaction mass making described secondary response column outlet place reaches reaction end, and be driven in B level filter press through described liquid conduits by the second mortar pump and to be filtered, filtrate after described B level sheet frame Filter Press is entered in product receiving slit by described liquid conduits, obtains thick product；
4) the thick product (chloride solid) separated regularly is put in alkali liquor, control the concentration of alkali liquor at 5～15mol/L simultaneously, after agitated and stratification, upper organic layer is collected, go to reclaim product, lower floor's material runs out after being centrifuged and reclaims chloride solid, and Recycling Mother Solution uses；
5) reaction end gas produced after described first order reaction post and described secondary response post react is reclaimed by gas conduit inflow water-jet vacuum pump, recycles after making ammonia.
2. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 1, it is characterized in that: step 2) and step 3) in described A level filter press and described B level filter press all include bracing frame, fixing tailgate, movable plate and locking device, described fixing tailgate is fixedly connected on support frame as described above, described movable plate is positioned at the end of described fixing tailgate, described movable plate connects described locking device, and described locking device is erected on support frame as described above.
3. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 2, it is characterized in that: the both sides up and down of described fixing tailgate are provided with water conservancy diversion cavity, the end of the described water conservancy diversion cavity being positioned below is provided with stock solution import, the end of described water conservancy diversion cavity above is provided with filtrate (liquid, it is evenly arranged with screen plate between two described water conservancy diversion cavitys, being evenly arranged with filtering holes on described screen plate, the two ends up and down of described screen plate connect described water conservancy diversion cavity respectively through drain pipe and feed tube.
4. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 2, it is characterised in that: described locking device includes handwheel and extrusion spring, and described handwheel connects described movable plate by described extrusion spring.
5. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 1, it is characterised in that: step 2) in described first order reaction post liquid level is described first order reaction post height 4/5.
6. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 1, it is characterised in that: step 3) in described secondary response post liquid level is described secondary response post height 3/4.
7. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 1, it is characterised in that: step 4) in time of described stratification be 5～10min.
8. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 1, it is characterised in that: step 4) in described alkali liquor be sodium hydroxide solution.
9. a kind of hexamethyldisiloxane pillar method for continuously synthesizing according to claim 1, it is characterized in that: step 5) in described water-jet vacuum pump include condenser pump, check-valves and tail pipe, described tail pipe is fixedly connected on the lower section of described condenser pump, described check-valves is fixedly connected on the side of described condenser pump, and the end of described check-valves is provided with vacuum meter.
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| CN106883257A (en) * | 2017-01-19 | 2017-06-23 | 浙江硕而博化工有限公司 | Trim,ethylchlorosilane produces HMDS new technology |
| CN108659030A (en) * | 2018-07-14 | 2018-10-16 | 浙江大学 | A kind of reaction system and method for continuous production hexamethyldisilazane |
| CN108745265A (en) * | 2018-07-14 | 2018-11-06 | 浙江大学 | Reaction system and method with the continuous production HMDS for strengthening mass transfer and flowing |
| CN109627446A (en) * | 2018-12-29 | 2019-04-16 | 中国船舶重工集团公司第七八研究所 | A kind of preparation facilities of polysilazane and preparation method thereof |
| CN109748932A (en) * | 2019-01-09 | 2019-05-14 | 浙江新化化工股份有限公司 | A kind of continuous synthesis method of hexamethyldisilazane |
| CN109776596A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The preparation method of 1,3- divinyl -1,1,3,3- tetramethyl-disilazane |
| CN112442061A (en) * | 2020-12-08 | 2021-03-05 | 江西贝特利新材料有限公司 | Silazane water washing method |
| CN114507253A (en) * | 2022-01-20 | 2022-05-17 | 杭州四马化工科技有限公司 | Continuous production process of silazane |
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| CN106883257A (en) * | 2017-01-19 | 2017-06-23 | 浙江硕而博化工有限公司 | Trim,ethylchlorosilane produces HMDS new technology |
| CN109776596A (en) * | 2017-11-14 | 2019-05-21 | 石家庄圣泰化工有限公司 | The preparation method of 1,3- divinyl -1,1,3,3- tetramethyl-disilazane |
| CN108659030A (en) * | 2018-07-14 | 2018-10-16 | 浙江大学 | A kind of reaction system and method for continuous production hexamethyldisilazane |
| CN108745265A (en) * | 2018-07-14 | 2018-11-06 | 浙江大学 | Reaction system and method with the continuous production HMDS for strengthening mass transfer and flowing |
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| CN109627446A (en) * | 2018-12-29 | 2019-04-16 | 中国船舶重工集团公司第七八研究所 | A kind of preparation facilities of polysilazane and preparation method thereof |
| CN109748932A (en) * | 2019-01-09 | 2019-05-14 | 浙江新化化工股份有限公司 | A kind of continuous synthesis method of hexamethyldisilazane |
| CN109748932B (en) * | 2019-01-09 | 2021-06-08 | 浙江新化化工股份有限公司 | Continuous synthesis method of hexamethyldisilazane |
| CN112442061A (en) * | 2020-12-08 | 2021-03-05 | 江西贝特利新材料有限公司 | Silazane water washing method |
| CN114507253A (en) * | 2022-01-20 | 2022-05-17 | 杭州四马化工科技有限公司 | Continuous production process of silazane |
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