CN201777994U - Alkylchlorosilane hydrolysis device - Google Patents
Alkylchlorosilane hydrolysis device Download PDFInfo
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- CN201777994U CN201777994U CN 201020517061 CN201020517061U CN201777994U CN 201777994 U CN201777994 U CN 201777994U CN 201020517061 CN201020517061 CN 201020517061 CN 201020517061 U CN201020517061 U CN 201020517061U CN 201777994 U CN201777994 U CN 201777994U
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- alkyl chlorosilane
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Abstract
The utility model relates to an alkylchlorosilane hydrolysis device comprising an enhanced mass transfer reactor, a gas condenser, a gas purifier, a phase separator and a storage tank, wherein a first opening and a second opening are arranged on the lateral surface of the reactor; a third opening is arranged at the top of the reactor; a fourth opening is arranged at the bottom of the reactor; the first opening is in fluid coupling with an alkylchlorosilane feeding pipe; the second opening is in fluid coupling with a saturated hydrochloric acid feeding pipe; the gas condenser is in fluid coupling with the reactor through the third opening; the gas purifier is in fluid coupling with the gas condenser; the bottom of the gas purifier is in fluid coupling with the reactor by a pipeline; a fifth opening is arranged at the top of the gas purifier; the phase separator is in fluid coupling with the reactor through the fourth opening; a sixth opening is arranged at the top of the phase separator; and the storage tank is in fluid coupling with the bottom of the phase separator by a pipeline and is in fluid coupling with the reactor through the saturated hydrochloric acid feeding pipe and the second opening. The utility model greatly improves the hydrolysis efficiency, improves the quality of hydrolysis products and saves the material and energy consumption.
Description
Technical field
The utility model belongs to chemical field, is specifically related to a kind of hydrolysis device of alkyl chlorosilane.
Background technology
The hydrolytic condensation method is to produce the most important a kind of method of organopolysiloxane by alkyl chlorosilane.
The alkyl chlorosilane hydrolysis generates alkylsilanol and hydrogenchloride, and it reacts this as thermo-negative reaction, but because the big calorimetric of HX generation soluble in water, so make alkyl chlorosilane be hydrolyzed to exothermic process.The speed of organosilane hydrolysis reaction strengthens and quantity is accelerated with Si-X key polarity, but increases and slow down with increase of organic radical steric hindrance and quantity.Alkyl chlorosilane during hydrolysis, can obtain the end capped polysiloxane of chlorine in the not enough water yield.
The finished product that the hydrolytic condensation of simple function group chlorosilane obtains are R3SiOSiR3, and reaction signal formula is as follows:
2R
3SiCl+2H
2O→2R
3SiOH+2HCl (1)
2R
3SiOH→2R
3SiR
3+H
2O (2)
The Me2Si (OH) 2 that the hydrolytic condensation of difunctionality chlorosilane (with dimethyldichlorosilane(DMCS), Me2SiCl2 is an example, is called for short diformazan) obtains, advanced intermolecular condensation generates the linear siloxane of low polymerization degree.The latter can carry out intermolecular and intramolecular two kinds of polyreactions, and finally obtaining linear polydiorganosiloxane [HO (Me2SiO) nH] and ring-type poly-two respectively has silicon machine oxygen alkane [(Me2SiO) n] two class products.Reaction formula is schematically as follows:
nMe
2SiCl
2+2nH
2O→nMe
2Si(OH)
2+2nHCl (3)
nMe
2Si(OH)
2→HO(Me
2SiO)nH+(n-1)H
2O (4)
nMe
2Si(OH)
2→(Me
2SiO)n+nH
2O (5)
The Me2SiCl2 hydrolysis-condensation reaction divides two stages to carry out, and promptly generates Me2SiClOH and Me2Si (OH) 2 earlier, and under proton-effect, self and condensation reaction each other further take place for they, form the SiOSi key.Shang Ruo hydrolysis or reaction conditions in not enough water gaging is too gentle, then can obtain α, ω-dichloro polydimethylsiloxane [ClMe2SiO (Me2SiO) nSiMe2Cl].
The hydrolytic condensation of trifunctional chlorosilane, according to the hydrolytic condensation processing condition, can generate linear organopolysiloxane, cyclic organic siloxane, loop wire organic silicon oxygen alkane, the build organo-siloxane that contains the Si-OH key and contain the crosslinking silicone of ring texture and the organopolysiloxane of three-dimensional network etc.
The hydrolytic condensation of four sense chlorosilanes, reaction process are very complicated, finally generate the SiO2 gel.
The alkyl chlorosilane hydrolyzate is colourless transparent liquid, and is flammable, and free from extraneous odour is water insoluble, is dissolved in organic solvents such as benzene.Be mainly used in and carry out the silicone oil that ring-opening polymerization becomes different polymerization degree, silicon rubber etc. also have a small amount of directly application.
Organosilicon material is of a great variety, ever-changing, mainly is divided into four big classes: silicone oil, silicon rubber, silicone resin and silane (comprising silane coupling agent and silica-basedization reagent).The preparation process of many organosilicon materials all is to be that raw material prepares polymethyl siloxane (base polymer) through hydrolysis with the methyl chlorosilane earlier, introduce other group such as phenyl, vinyl, chloro-phenyl-, Qing Wanji, fluoroalkyl etc. again, make it possess special nature and function.
The chlorosilane hydrolysis process has excessive water hydrolysis process and azeotropic acid hydrolysis technology, generates the wire polysiloxane of end group hydroxyl and the hydrolyzate and the hydrochloric acid of cyclic polysiloxanes.To emit a large amount of heat because hydrolysis generates in the water-soluble or diluted acid of hydrogenchloride,, then need keep the hydrolysis reaction technological temperature, promptly heat should be shifted out if obtain the vast scale cyclic polysiloxanes.The concentration of hydrochloric acid differences that two kinds of methods generate, the hydrogenchloride that obtains being used for the synthetic methyl chloride of methyl alcohol all needs to take off analyses operation, has increased equipment and energy expenditure.
Saturated hydrochloric acid and chlorosilane water generation reaction are separated thing, saturated hydrochloric acid and hydrogenchloride, but still have the hydrogenchloride about 30% to exist with the form of saturated hydrochloric acid, and this method still needs to take off analyses the hydrogenchloride operation, also can increase equipment and energy expenditure.
Concentrated acid hydrolysis: the ordinary-pressure hydrolysis of recycle acid concentration 36%-37%, though recycle acid concentration can reach the hydrogenchloride that 40%-50% pressurization concentrated acid hydrolysis process method solved increase equipment and energy expenditure and take off the problems referred to above such as analysing operation, but situation about existing in the actual production is: 0.139535 ton of water of dimethylchlorosilane hydrolysis needs per ton produces about 0.55 ton of hydrogenchloride.Chlorosilane runs into water hydrolysis reaction just takes place, and the hydrogenchloride of generation does not have water dissolution to overflow with gas form.Though the chlorosilane hydrolysis reaction is irreversible, hydrolysis reaction can not be carried out because chlorine hydride gas concentration increases.But the problem that puzzlement is produced is:
1. under high hydrogen cloride concentration, the organochlorosilane particle surface can form one deck hydrogen chloride gas film, makes water molecules be difficult for fully contacting with the organochlorosilane molecule, thereby can reduce hydrolysis reaction speed.
Hydrolysis reaction fully before, the molecule of organochlorosilane will diffuse in the hydrogen chloride gas and be taken out of.Therefore, reduce the purity that yield also has influence on hydrogen chloride gas simultaneously, synthesize to methyl chloride and cause certain influence.
3. the concentrated acid hydrolysis also may produce terminal chloride linear siloxane, influences the quality of hydrolyzate, and then influences the quality of subsequent downstream product.
The saturated acid hydrolysis process of alkyl chlorosilane is to allow alkyl chlorosilane closed cycle hydrolysis in saturated acid (hydrochloric acid is in saturation concentration under the temperature and pressure condition that reaction requires).The used hydrochloric acid of saturated acid hydrolysis is in a kind of closed cycle state, just alkyl chlorosilane and the water in system, imported, output is hydrolyzate and gaseous hydrogen chloride, compares the amount of carrying secretly of hydrolyzate when having reduced hydrochloric acid output with azeotropic acid hydrolysis technology, so the yield of hydrolyzate is higher; Energy consumption during the coproduction methyl chloride also descends greatly.
Hydrolysis reaction has nothing in common with each other, and patent CN101323666A discloses the method for a kind of chloromethyl-dimethylchlorosilane hydrolysis, directly chloromethyl-dimethylchlorosilane is dripped in water, and the reaction that is hydrolyzed utilizes this reaction self heat release can finish reaction.
Use packing tower alkyl chlorosilane hydrolysis reactor among the CN101323666A; Patent US5169970 is in the stirring tank reaction that is hydrolyzed, and stirred autoclave efficient is low, mixes inhomogeneously, in order to reach the enough reaction times, must strengthen its volume, be unfavorable for serialization production, and technological operation elasticity is little; The patent US2008/0154055 A1 reaction that in the sequence of constant boiling and rectification tower, is hydrolyzed.
Above process exists following problem, and two reactants of water and alkyl chlorosilane contact inhomogeneous, and alkyl chlorosilane residence time in reactor is long and distribute very widely, and otherness is very big each other to cause the polymerization degree of oxosilane and molecular conformation.
Patent CN1712429A and the CN1108267A reaction that in annular reactor, is hydrolyzed; The first step wherein is lower than in density in the presence of 0.9 the water-insoluble organic solvents, and with respect to every mole of hydrolyzable chlorine, the mol ratio of alkyl chlorosilane and water is 2: 1.
Patent US4609751 saturated acid hydrolysis reaction divides multistage carrying out, alkyl chlorosilane is after the one-stage hydrolysis recycle system is through static mixer reaction and phase separator, obtain gas phase chlorination hydrogen with pressure, gas phase chlorination hydrogen can be directly used in synthetic methyl chloride or water and absorb and make industrial hydrochloric acid after overcooling oil removing, decon and drying.
Above process existing problems are, gaseous state HCl can not in time overflow from solution in the product of alkyl chlorosilane hydrolysis, on the one hand, under high HCl concentration, can form the HCl air film on the surface of alkyl chlorosilane, hindered water and contacted with it, therefore reduced speed of response, also can cause the oxosilane chlorinity to increase on the other hand, increase the burden of postorder dechlorination process, increase material consumption and energy consumption greatly.
Because the hydrolysis reaction of alkyl chlorosilane is the rapid reaction process, so the quick uniform mixing of alkyl chlorosilane and water, and in time will reacts the gas HCl that produces and shift out, just very important.So wishing has a kind of alkyl chlorosilane hydrolysis device to overcome the defective of prior art.
The utility model content
Technical problem to be solved in the utility model is: low at the conversion unit stirring efficiency that exists in the above process, mix inhomogeneous, long reaction time, product purity is low, and the big shortcoming of material consumption energy consumption, provide a kind of alkyl chlorosilane hydrolysis device, in order to improve hydrolysis reaction efficient, improve the quality of hydrolysate, reduce material consumption and energy consumption simultaneously.
Technical problem to be solved in the utility model is solved by the following technical programs:
A kind of alkyl chlorosilane hydrolysis device is characterized in that, comprising:
One reinforcing mass transfer reactor, described reactor side is provided with first opening and second opening, and the top is provided with the 3rd opening, and the bottom is provided with the 4th opening; Described first opening is connected with alkyl chlorosilane feed-pipe fluid; Described second opening is connected with saturated hydrochloric acid feed-pipe fluid;
The gas condenser that is connected with described reactor fluid by the 3rd opening;
The gas purifier that is connected with described gas condenser fluid; Described gas purifier bottom is connected with described reactor fluid by pipeline, and the top is provided with the 5th opening;
The phase separator that is connected with described reactor fluid by the 4th opening; Described phase separator top is provided with the 6th opening; With
The storage tank that is connected with the phase separator bottom flow by pipeline; Described storage tank is connected with reactor fluid by saturated hydrochloric acid feed-pipe, second opening.
Described inside reactor can be provided with a liquid distributor and be positioned at the rotor of described liquid distributor inside, is filled with filler in the described rotor.
Described liquid distributor can be two liquid jet or shower nozzle or the static mixers that spray relatively.
Filler can be wire packing, dumped packing, the structured packing of twining in the described rotor, and its material can be the metallic substance Hastelloy, tantalum, zirconium etc., or Erosion-Resisting Non-metallic Materials such as poly-fluorohydrocarbon class.
During use, alkyl chlorosilane and saturated hydrochloric acid enter in the reinforcing mass transfer reactor by first opening and second opening respectively, two strands of liquid materials are after the preliminary fast mixing of liquid distributor, the high speed rotating filler cutting that is reinforced the rotor inner edge in the mass transfer reaction device breaks up, and is dispersed into minimum drop and collides contact reacts each other.These drops are under action of centrifugal force, further collide, atomize with adjacent following one deck filler, reaction rapidly in the collision process so repeatedly, products therefrom finally leaves the rotor outer rim, after the collision of equipment inwall, flow out the reinforcing mass transfer reactor by the 4th opening rapidly.
The liquid product of reaction in time enters phase separator by the 4th opening, in phase separator siloxanes is separated with hydrochloric acid.Isolated saturated hydrochloric acid is stored in the storage tank, in order to getting back to the reinforcing mass transfer reactor as raw material later on.
The HCl gas that process produces promotes because of pressure reduction, in time from liquid, overflow, after passing the packing layer arrival its upper side freeboard of rotation, leave from the 3rd opening of efficient reinforcing mass transfer gas reactor, behind gas condenser and gas purification utensil, obtain being used to produce the hydrogen chloride gas of methyl chloride, condensation is reclaimed volatile alkyl chlorosilane and is got back to the reinforcing mass transfer reactor.The clean gaseous state HCl that removes moisture and low volatilization siloxanes gets back to leading portion building-up reactions operation and uses as raw material.
Alkyl chlorosilane hydrolysis device of the present utility model, owing to adopted the reinforcing mass transfer reactor, through preliminary mixed liquid material, broken up by the cutting of the high speed rotating filler of the rotor inner edge in the equipment, and collide contact reacts each other, the alkyl chlorosilane hydrolysis reaction is evenly carried out, and in time will react the gas HCl that produces and shift out, therefore improve hydrolytic process efficient greatly, and because material is at the reactor residence time narrowly distributing, so the molecular conformation of product and molecular weight distribution are very regular, and the cl content of hydrolysate is also lower, thereby improved the quality of hydrolysate, saved the material consumption and the energy consumption of later stage dechlorination and purifying.
Description of drawings
Below in conjunction with the drawings and specific embodiments the utility model is described further.
Fig. 1 is the hydrolysis device and the hydrolysis process schema of alkyl chlorosilane of the present utility model.
Embodiment
In order to make technique means of the present utility model, creation characteristic, to reach purpose and effect is easy to understand, below in conjunction with embodiment, further set forth the utility model, but embodiment of the present utility model is not limited thereto.
Embodiment 1
As shown in Figure 1, a kind of alkyl chlorosilane hydrolysis device comprises:
One reinforcing mass transfer reactor 1, described reactor 1 inside are provided with a liquid distributor 2 and are positioned at the rotor 3 of described liquid distributor inside; Described reactor side is provided with first opening 11 and second opening 12, and described reactor head is provided with the 3rd opening 13, and the bottom is provided with the 4th opening 14; Be filled with filler (black part among the figure) in the described rotor; Described first opening 11 is connected with alkyl chlorosilane feed-pipe 16 fluids; Described second opening 12 is connected with saturated hydrochloric acid feed-pipe fluid 15;
The gas condenser 4 that is connected with described reactor 1 fluid by the 3rd opening 13;
The gas purifier 5 that is connected with described gas condenser 4 fluids; Described gas purifier 5 bottoms are connected with described reactor 1 fluid by pipeline, and the cleaner top is provided with the 5th opening 51;
The phase separator 6 that is connected with described reactor 1 fluid by the 4th opening 14; Described phase separator 6 tops are provided with the 6th opening 61; With
The salt acid storage tank 7 that is connected with phase separator 6 bottom flow by pipeline; Described storage tank 7 is connected with reactor 1 fluid by saturated hydrochloric acid feed-pipe 15, second opening 12.
The tantalum wire net of filler for twining in the rotor of reinforcing mass transfer reactor.
During use, alkyl chlorosilane and saturated hydrochloric acid enter in the reinforcing mass transfer reactor 1 by first opening 11 and second opening 12 respectively, two strands of liquid materials are after the preliminary fast mixing of liquid distributor 2, the high speed rotating filler cutting that is reinforced rotor 3 inner edges in the mass transfer reaction device 1 breaks up, and is dispersed into minimum drop and collides contact reacts each other.These drops are under action of centrifugal force, further collide, atomize with adjacent following one deck filler, reaction rapidly in the collision process so repeatedly, products therefrom finally leaves the rotor outer rim, after the collision of equipment inwall, flow out reinforcing mass transfer reactor 1 by the 4th opening 14 rapidly.
The liquid product of reaction in time enters phase separator 6 by the 4th opening 14, in phase separator 6 siloxanes is separated with hydrochloric acid.Isolated saturated hydrochloric acid is stored in the storage tank 7, in order to getting back to reinforcing mass transfer reactor 1 as raw material later on.
The HCl gas that process produces promotes because of pressure reduction, in time from liquid, overflow, after passing the packing layer arrival its upper side freeboard of rotation, leave from the 3rd opening 13 of efficient reinforcing mass transfer reactor 1, after gas condenser 4 and gas purifier 5 purifications, obtain being used to produce the hydrogen chloride gas of methyl chloride, condensation is reclaimed volatile alkyl chlorosilane and is got back to reinforcing mass transfer reactor 1.The clean gaseous state HCl that removes moisture and low volatilization siloxanes gets back to the leading portion synthesis procedure and uses as raw material.
More than show and described ultimate principle of the present utility model, principal character and advantage of the present utility model.The technician of the industry should understand; the utility model is not restricted to the described embodiments; that describes in the foregoing description and the specification sheets just illustrates principle of the present utility model; the utility model also has various changes and modifications under the prerequisite that does not break away from the utility model spirit and scope, and these changes and improvements all fall in claimed the utility model scope.The claimed scope of the utility model is defined by appending claims and equivalent thereof.
Claims (5)
1. an alkyl chlorosilane hydrolysis device is characterized in that, comprising:
One reinforcing mass transfer reactor, described reactor side is provided with first opening and second opening, and the top is provided with the 3rd opening, and the bottom is provided with the 4th opening; Described first opening is connected with alkyl chlorosilane feed-pipe fluid; Described second opening is connected with saturated hydrochloric acid feed-pipe fluid;
The gas condenser that is connected with described reactor fluid by the 3rd opening;
The gas purifier that is connected with described gas condenser fluid; Described gas purifier bottom is connected with described reactor fluid by pipeline, and the top is provided with the 5th opening;
The phase separator that is connected with described reactor fluid by the 4th opening; Described phase separator top is provided with the 6th opening; With
The storage tank that is connected with the phase separator bottom flow by pipeline; Described storage tank is connected with reactor fluid by saturated hydrochloric acid feed-pipe, second opening.
2. a kind of alkyl chlorosilane hydrolysis device as claimed in claim 1 is characterized in that, described inside reactor is provided with a liquid distributor and is positioned at the rotor of described liquid distributor inside, is filled with filler in the described rotor.
3. a kind of alkyl chlorosilane hydrolysis device as claimed in claim 2 is characterized in that, described liquid distributor is two liquid jet or the shower nozzles that spray relatively.
4. a kind of alkyl chlorosilane hydrolysis device as claimed in claim 2 is characterized in that described liquid distributor is a static mixer.
5. a kind of alkyl chlorosilane hydrolysis device as claimed in claim 2 is characterized in that, filler is wire packing, dumped packing or the structured packing of twining in the described rotor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201020517061 CN201777994U (en) | 2010-09-02 | 2010-09-02 | Alkylchlorosilane hydrolysis device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201020517061 CN201777994U (en) | 2010-09-02 | 2010-09-02 | Alkylchlorosilane hydrolysis device |
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| CN201777994U true CN201777994U (en) | 2011-03-30 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382305A (en) * | 2010-09-02 | 2012-03-21 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN102492144A (en) * | 2011-12-09 | 2012-06-13 | 上海安赐机械设备有限公司 | Saturated acid hydrolysis technology of alkylchlorosilane |
| CN103011527A (en) * | 2012-12-29 | 2013-04-03 | 上海安赐机械设备有限公司 | Enhanced oxidation-MBR (membrane bioreactor) treatment method of caprolactam production wastewater |
| CN106317095A (en) * | 2016-08-16 | 2017-01-11 | 湖北兴发化工集团股份有限公司 | Hydrolysis technology and device for concentrated hydrochloric acid |
-
2010
- 2010-09-02 CN CN 201020517061 patent/CN201777994U/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102382305A (en) * | 2010-09-02 | 2012-03-21 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN102382305B (en) * | 2010-09-02 | 2013-01-02 | 上海安赐机械设备有限公司 | Alkyl chlorosilane hydrolysis device and hydrolysis process thereof |
| CN102492144A (en) * | 2011-12-09 | 2012-06-13 | 上海安赐机械设备有限公司 | Saturated acid hydrolysis technology of alkylchlorosilane |
| CN102492144B (en) * | 2011-12-09 | 2014-03-12 | 上海安赐机械设备有限公司 | Saturated acid hydrolysis technology of alkylchlorosilane |
| CN103011527A (en) * | 2012-12-29 | 2013-04-03 | 上海安赐机械设备有限公司 | Enhanced oxidation-MBR (membrane bioreactor) treatment method of caprolactam production wastewater |
| CN106317095A (en) * | 2016-08-16 | 2017-01-11 | 湖北兴发化工集团股份有限公司 | Hydrolysis technology and device for concentrated hydrochloric acid |
| CN106317095B (en) * | 2016-08-16 | 2018-09-07 | 湖北兴发化工集团股份有限公司 | A kind of concentrated hydrochloric acid hydrolysis technique and device |
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| GR01 | Patent grant | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20110330 Effective date of abandoning: 20130227 |
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| RGAV | Abandon patent right to avoid regrant |