CN202705272U - Device for preparing tetramethyldihydrodisiloxane - Google Patents

Device for preparing tetramethyldihydrodisiloxane Download PDF

Info

Publication number
CN202705272U
CN202705272U CN 201220371302 CN201220371302U CN202705272U CN 202705272 U CN202705272 U CN 202705272U CN 201220371302 CN201220371302 CN 201220371302 CN 201220371302 U CN201220371302 U CN 201220371302U CN 202705272 U CN202705272 U CN 202705272U
Authority
CN
China
Prior art keywords
feed
discharge port
opening
tetramethyl
hydrochloric acid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
CN 201220371302
Other languages
Chinese (zh)
Inventor
谭军
薛常洪
欧阳玉霞
程旭阳
鄢清佳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JIAXING UNITED CHEMICAL CO Ltd
Jiaxing University
Original Assignee
JIAXING UNITED CHEMICAL CO Ltd
Jiaxing University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by JIAXING UNITED CHEMICAL CO Ltd, Jiaxing University filed Critical JIAXING UNITED CHEMICAL CO Ltd
Priority to CN 201220371302 priority Critical patent/CN202705272U/en
Application granted granted Critical
Publication of CN202705272U publication Critical patent/CN202705272U/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Abstract

The utility model discloses a device for preparing tetramethyldihydrodisiloxane. The device comprises a hydrolysis reaction kettle, a phase separation device, a first control valve, a washing kettle and a rectification device, wherein the hydrolysis reaction kettle is provided with a diluted hydrochloric acid feeding hole and a dimethylhydrochlorosilane feeding hole; a feeding hole of the phase separation device is communicated with a discharge hole of the hydrolysis reaction kettle; the first control valve is arranged on a pipeline between the discharge hole of the hydrolysis reaction kettle and the feeding hole of the phase separation device; a feeding hole of the washing kettle is communicated with an organic phase discharge hole of the phase separation device, and the washing kettle is provided with a washing water feeding hole; and a feeding hole of the rectification device is communicated with a discharge hole of the washing kettle. The device for preparing the tetramethyldihydrodisiloxane is easy to operate; other organic solvents are not required in the whole preparation process, the produced hydrogen chloride can be recycled, and the tetramethyldihydrodisiloxane serving as a final product obtained after a crude product is rectified is high in yield and high in quality; and the operation steps are simple, the safety and the process stability are high, the energy consumption is low, and industrialization is easy to realize.

Description

The device of preparation tetramethyl-dihydro sily oxide
Technical field
The utility model belongs to the organosilane monomer production technical field, is specifically related to a kind of device for preparing tetramethyl-dihydro sily oxide.
Background technology
Organosilicon material mainly be a class take the Si-O key as main chain, on Si, introduce again organic group as the macromolecular compound of side chain, its excellent performance, function are unique.Since 21 century, organosilicon material is widely used in military technology, building industry, textile industry, chemical industry, metal and paint industry, medical medical treatment, electric industry, and the field such as space flight and aviation, be listed in one of industry of state key encourage growth.Organochlorosilane is the main raw material that is prepared with organosilicon polymer material and other functional silane.Therefore, the production status of organochlorosilane has determined the height of a national Silicone Industry level to a great extent.
Tetramethyl-dihydro sily oxide, molecular formula are HMe 2SiOSiMe 2H, full name 1,1,3,3 ,-tetramethyl--1,3-dihydro sily oxide is commonly called as hydrogeneous double-seal head.A kind of excellent performance, the fine chemicals that of many uses, added value is high, the especially large extraordinary reactive intermediate of a kind of interrelationship between industries.Because the reactive hydrogen on its two end group has advantageous condition in research and industrial application.It utilizes the Si-H key on its end group as producing organic-silicon-modified block or the crucial starting raw material of graft copolymer and important silicone intermediate, by hydrosilation reaction, can introduce various organic groups at the polysiloxane molecule chain; So end hydrogen based polysiloxane is at modified plastics, resin modified, in silicon oil modified, the linking agent of liquid silastic, extraordinary organic silicon surfactant and branch-shape polymer synthetic important purposes is arranged.But the purity of tetramethyl-dihydro sily oxide, chloride ion content are very large on its application impact in the organosilicon Downstream Products, and the purity of superior product generally need to be more than 99%, and chlorion is then at 10 below the ppm.
At present, the topmost synthesis technique of tetramethyl-dihydro sily oxide is mainly by dimethyl silicane hydroxide (Me 2HSiCl) hydrolysis, rectifying preparation.General water and the organic solvent of adopting is as reaction medium in the hydrolytic process, and production cost is higher and environmental pollution is comparatively serious.And the polycondensation side reaction easily occurs in the tetramethyl-dihydro sily oxide that obtains behind the hydrolysis reaction, and the yield of target product is lower.
In addition, dimethyl silicane hydroxide (Me 2HSiCl) purity difference and hydrolysis process condition are different, all can considerable influence be arranged to hydrolysis purpose product tetramethyl-dihydro sily oxide yield and purity.The patent of invention CN101544666B that Jiaxing Joint Chemical Co., Ltd obtains the authorization reported a kind of from low-boiling-point substance the method for purification dimethyl silicane hydroxide.Mainly by adding extraction agent, the by-product low-boiling-point substance that industrial direct method is produced in the methyl chlorosilane carries out separation of extractive distillation to the method.Wherein extraction agent is that boiling point is not less than 70 ℃ polar aprotic solvent.The extraction rectifying method that this invention is adopted is with Me 2The hydrocarbon polymer 2-methyl-2-butene effective separation that HSiCl and boiling point are close, thus Me in the conventional rectification method of purification broken 2HSiCl purity can only reach 88% limitation, realizes Me in the cut 2HSiCl content is more than 95%.The method provides purer raw material Me for the purer tetramethyl-dihydro sily oxide of preparation 2HSiCl.
Other preparation methods about tetramethyl-dihydro sily oxide mainly contain: the people such as Zhang Qunchao (Wuhan University Journal Edition, 2007,53 (2): 175~178) make the monosubstituted ethoxy dimethylchlorosilane with dimethyldichlorosilane(DMCS) and ethanol gas and liquid phase alcoholysis reaction, then add catalyst Fe Cl 3Back flow reaction makes intermediate dihydro tetramethyl disiloxane, further uses CaH in anhydrous diethyl ether 2The reduction intermediate obtains tetramethyl disiloxane, and productive rate is up to 86%.But from existing technical Analysis, this method production cost is obviously too high, has used dangerous higher ether solvent in the reaction process, is difficult to industrial applications.
The utility model content
The utility model provides a kind of device for preparing tetramethyl-dihydro sily oxide, and this apparatus structure is simple, and is easy to operate, utilizes this device can realize the recycling of dilute hydrochloric acid, and preparation cost is low, environmental friendliness.
A kind of device for preparing tetramethyl-dihydro sily oxide comprises:
Hydrolytic reaction pot with dilute hydrochloric acid opening for feed and dimethyl silicane hydroxide opening for feed;
The phase-separating device that opening for feed is communicated with the discharge port of hydrolytic reaction pot;
Be located at the first control valve on the pipeline between the opening for feed of the discharge port of hydrolytic reaction pot and phase-separating device;
The washing kettle that opening for feed is communicated with the organic phase discharge port of phase-separating device, on the washing kettle with the washing water opening for feed;
The rectifier unit that opening for feed is communicated with the discharge port of washing kettle.
In the said apparatus operational process, affect carrying out smoothly of subsequent job for preventing from reacting the solid impurity that mixes in the fixedly impurity that self produces or the reaction process, a kind of preferred technical scheme is: the pipeline between the discharge port of described the first control valve and the opening for feed of phase-separating device is provided with strainer, before material enters phase-separating device, the fixedly impurity that contains in the material is removed, prevented this fixedly follow-up phase-separating device and rectifier unit of impurity obstruction.
In the said apparatus, for reducing production costs, realize the recycling of raw material, described phase-separating device is preferably the liquid-liquid phase separation device, and the inorganic phase discharge port of liquid-liquid phase separation device is communicated with the dilute hydrochloric acid opening for feed of hydrolytic reaction pot.
For guaranteeing Systems balanth, as further preferred, pipeline between the dilute hydrochloric acid opening for feed of described hydrolytic reaction pot and the inorganic phase discharge port of liquid-liquid phase separation device is provided with the dilute hydrochloric acid storage tank, and pipeline is provided with the second control valve between the dilute hydrochloric acid opening for feed of this dilute hydrochloric acid storage tank discharge port and hydrolytic reaction pot.The setting of dilute hydrochloric acid storage tank, avoid since the fluctuation of subsequent job on the impact of dilute hydrochloric acid add-on in the hydrolytic reaction pot.
The control of the amount that adds for ease of dimethyl silicane hydroxide, as preferably, also comprise the dimethyl silicane hydroxide storage tank, the dimethyl silicane hydroxide opening for feed of described hydrolytic reaction pot is communicated with the discharge port of this dimethyl silicane hydroxide storage tank, and pipeline between the two is provided with the 3rd control valve.
Control for ease of the water yield in the washing kettle, another kind of preferred technical scheme is: also comprise the deionized water hold-up vessel, the washing water opening for feed of described washing kettle is communicated with the discharge port of this deionized water storage tank, pipeline between the two is provided with the 4th control valve, can be by the 4th control valve control washing amount and washing speed.
Described rectifier unit can be selected material filling type rectifying tower or plate distillation column, for ease of design and control, as preferably, described rectifier unit is plate distillation column, the plate distillation column cat head is provided with condenser, and the material part that condensation obtains is collected as front-end volatiles; Being tetramethyl-dihydro sily oxide discharge port in the tower, is a small amount of oligopolymer discharge port at the bottom of the tower.
First, second, third, fourth and fifth described in the utility model only are in order to distinguish and identify a plurality of control valves, are not the restriction to the construction features of control valve own or annexation, and implication does not sort yet.Described control valve can be selected check valve or two-way valve, can adopt manual valve also can adopt motorized valve, is prior art, can select according to actual needs.
For further describing, the utility model provides a kind of preparation method of tetramethyl-dihydro sily oxide, the method utilizes dimethyl silicane hydroxide to be raw material, make tetramethyl-dihydro sily oxide through hydrolysis, avoid adopting the reaction solvent of high poison, high-risk, environmental friendliness, simple to operate, be easy to realize industrialization.
A kind of preparation method of tetramethyl-dihydro sily oxide comprises: the dimethyl silicane hydroxide raw material is joined the reaction that is hydrolyzed in the dilute hydrochloric acid, and hydrolysis reaction is finished, and aftertreatment obtains tetramethyl-dihydro sily oxide; The mass percent concentration of hydrogenchloride is 5-20% in the described dilute hydrochloric acid, and described hydrolysising reacting temperature is 0-60 ℃; The reaction process of above-mentioned reaction is shown below:
2Me 2SiHCl+H 2O→HMe 2SiOSiMe 2H+2HCl
In the above-mentioned reaction process, be further to reduce post-processing difficulty, reduce side reaction, improved the purity of product, as preferably, the mass percentage content of dimethyl silicane hydroxide is greater than 95% in the described dimethyl silicane hydroxide raw material.Can select the commercially available prod, also can adopt existing method preparation, the Granted publication number method preparation for providing among the CN101544666B for example can be provided.
In the above-mentioned reaction, the effect major embodiment of dilute hydrochloric acid both ways: on the one hand the hydrolysis for dimethyl silicane hydroxide provides the acidic hydrolysis environment; Play on the other hand the effect of stopper: can produce HCl in the hydrolytic process of dimethyl silicane hydroxide, adding dilute hydrochloric acid can reduce the severe degree of hydrolysis reaction, prevent because the too fast temperature of reaction system that causes of reaction is too high, and then cause tetramethyl-dihydro sily oxide that the polycondensation side reaction occurs under hot conditions.The concentration of dilute hydrochloric acid can not be too high, and during excessive concentration, the hydrolysis reaction resistance is excessive, and what be unfavorable for reacting carries out smoothly.As further preferred, the mass percent concentration of hydrogenchloride is 10~15% in the described dilute hydrochloric acid.
In the said hydrolyzed reaction, the temperature of hydrolysis reaction is unsuitable too high, and too high meeting causes the generation of tetramethyl-dihydro sily oxide polycondensation side reaction, has reduced the ultimate yield of tetramethyl-dihydro sily oxide.Further preferred hydrolysising reacting temperature is 0~30 ℃, and the hydrolysis time general control was at 2~10 hours, and the concrete reaction times can be determined according to the real reaction situation.
For guaranteeing carrying out smoothly of said hydrolyzed reaction, the volume ratio of the adding of described dimethyl silicane hydroxide raw material and dilute hydrochloric acid is 1:4~1:10, and preferred volume ratio is 1:5~1:8.The excessive difficulty that increases aftertreatment of the volume of the adding of dilute hydrochloric acid is unfavorable for the carrying out of aftertreatment.
After reaction was finished, the product of reaction was hydrogenchloride, tetramethyl-dihydro sily oxide and a small amount of oligopolymer, and described last handling process is:
(1) with reacting liquid filtering: remove the solid impurity that produces in the reaction process or mix because of carelessness, avoid solid impurity to the detrimentally affect of subsequent disposal;
(2) filtration is obtained the filtrate layering: hierarchical operations can adopt the phase separator standing demix, lower floor is the inorganic phase of the hydrochloric aqueous solution after the layering, the upper strata is the organic phase that contains the siloxanes crude product, lower floor's hydrochloric acid water is separated in phase separator, but the hydrolysis stopper is made in reuse after the waste hydrochloric acid dilution;
(3) organic phase that layering is obtained is washed to neutrality: washing operation can carry out in washing kettle;
(4) the thick product after will washing carries out rectifying and obtains that purity is more than 99.5%, the tetramethyl-dihydro sily oxide of chloride ion content below 10ppm, and a small amount of low-boiling-point substance and oligopolymer then reuse are done other products.
The device of preparation tetramethyl-dihydro sily oxide of the present utility model, one-piece construction is simple, utilize in this device preparation tetramethyl-dihydro sily oxide whole process and need not other organic solvents, capable of circulation the applying mechanically of hydrogenchloride that produces, the finished product tetramethyl-dihydro sily oxide yield that crude product obtains after rectifying is higher, good product quality, and operation steps is simple, security and technology stability are all better, and energy consumption is lower, are easy to realize industrialization.
Description of drawings
Fig. 1 is preparation method's process flow diagram of tetramethyl-dihydro sily oxide of the present utility model;
Fig. 2 is the structural representation of the device of preparation tetramethyl-dihydro sily oxide of the present utility model;
Among Fig. 2:
Figure BDA00001946581900061
Embodiment
The utility model is described in further detail below in conjunction with drawings and Examples.Only as exemplary, can not limit content of the present utility model below should understanding.
Embodiment 1
Be described further below in conjunction with the device of accompanying drawing to preparation tetramethyl-dihydro sily oxide of the present utility model, as shown in Figure 2, comprise dilute hydrochloric acid storage tank 1, dimethyl silicane hydroxide storage tank 2, hydrolytic reaction pot 3, strainer 4, liquid-liquid phase separation device 5, washing kettle 7, condenser 8, front-end volatiles storage tank 9, tetramethyl-dihydro sily oxide storage tank 10, rectifying tower 11, containing hydrogen silicone oil storage tank 12, the first control valve 17, the second control valve 13, the 3rd control valve 14, the 4th control valve 15 and the 5th control valve 16.Contain chuck in the hydrolytic reaction pot 3, be convenient to the control to temperature in the kettle.Rectifier unit is plate distillation column.
The concrete annexation of each parts is: the dilute hydrochloric acid opening for feed of hydrolytic reaction pot 3 is communicated with the discharge port of dilute hydrochloric acid storage tank 1, and pipeline between the two is provided with the second control valve 13; The dimethyl silicane hydroxide opening for feed of hydrolytic reaction pot 3 is communicated with the discharge port of dimethyl silicane hydroxide storage tank 2, above-mentioned the 3rd control valve 14 that is provided with of pipeline between the two; Be provided with whipping appts in the hydrolytic reaction pot 3, represent with M among the figure, the discharge port of hydrolytic reaction pot 3 is communicated with the opening for feed of strainer 4, and pipeline between the two is provided with the second control valve 17; The discharge port of strainer 4 is communicated with the opening for feed of liquid-liquid phase separation device 5, and the organic phase discharge port of liquid-liquid phase separation device 5 is communicated with the material feeding mouth of washing kettle 7, and the inorganic phase discharge port of liquid-liquid phase separation device 5 is communicated with the opening for feed of dilute hydrochloric acid storage tank 1; The washing water opening for feed of washing kettle 7 is communicated with the water outlet of deionized water storage tank 6, pipeline between the two is provided with the 4th control valve 15, enter in the wastewater disposal basin 18 after the washing water discharge port neutralizing treatment of washing kettle 7, the discharge port of washing kettle 7 is communicated with the opening for feed of rectifying tower 11, also be provided with whipping appts in the washing kettle 7, represent with M equally; Rectifying tower 11 cats head are provided with condenser 8, the discharge port of condenser 8 is communicated with the cat head feedback outlet of rectifying tower 11 and the opening for feed of front-end volatiles storage tank 9 simultaneously, discharge port is communicated with tetramethyl-dihydro sily oxide storage tank 10 opening for feeds in rectifying tower 11 towers, and discharge port is communicated with containing hydrogen silicone oil storage tank 12 at the bottom of rectifying tower 11 towers.
The detailed process of the material in the said apparatus is: the reaction that is hydrolyzed in hydrolytic reaction pot 3 of dimethyl silicane hydroxide and dilute hydrochloric acid, product are hydrogenchloride, tetramethyl-dihydro sily oxide and a small amount of oligopolymer.After reaction finished, product was removed a small amount of solid impurity through filter 4.Product after the filtration carries out layering by liquid-liquid phase separation device 5, reuse is done the hydrolysis stopper after the isolated concentrated hydrochloric acid dilution of lower floor to hydrolytic reaction pot 3, and upper strata isolated tetramethyl-dihydro sily oxide crude product enters and repeatedly is washed to neutrality in the washing kettle 7.The tetramethyl-dihydro sily oxide crude product that will be again neutrality passes into and carries out rectifying in the rectifying tower 8, obtain purity and be the tetramethyl-dihydro sily oxide more than 99.5%, be collected in tetramethyl-dihydro sily oxide storage tank 10, a small amount of low-boiling-point substance is collected in front-end volatiles storage tank 9, and a small amount of oligopolymer is collected in containing hydrogen silicone oil storage tank 12.
Embodiment 2
(1) be that 98% dimethyl silicane hydroxide and mass percent concentration are that 10% dilute hydrochloric acid solution reacts in hydrolytic reaction pot with mass percentage content, hydrolysis temperature is controlled at about 10 ℃, reaction times is 3 hours, the volume ratio of dimethyl silicane hydroxide and dilute hydrochloric acid is 1:6, and reaction product is hydrogenchloride, tetramethyl-dihydro sily oxide and a small amount of oligopolymer.After reaction finished, product filtered, and removes a small amount of solid impurity.
(2) the hydrolysis crude product after the filtration enters the phase separator standing demix.Lower floor is the hydrochloric acid water after the layering, and the upper strata is siloxanes crude product phase, lower floor's hydrochloric acid water is separated in phase separator, but reuse is done the hydrolysis stopper after the waste hydrochloric acid dilution to step (1).
The tetramethyl-dihydro sily oxide crude product that (3) will obtain from phase separator is in washing kettle.Utilize deionized water repeatedly to wash, until the crude product system is neutral, the waste water after the washing is discharged wastewater disposal basin after neutralization.
(4) will be neutral tetramethyl-dihydro sily oxide crude product passes into and carries out rectifying in the rectifying tower, Rectification column pressure is controlled at normal pressure, temperature is controlled at 140~150 ℃, obtain the tetramethyl-dihydro sily oxide that purity is about 99.6%, chloride ion content is about 8ppm, a small amount of low-boiling-point substance front-end volatiles that rectifying obtains and containing hydrogen silicone oil by product then reuse are done other products.The final tetramethyl-dihydro sily oxide yield that calculates is about 95%.Schema as shown in Figure 1.
Dimethyl silicane hydroxide can adopt the commercially available prod, also can adopt Granted publication number to prepare for the preparation method of CN101544666B.
Embodiment 3
(1) be that 96% dimethyl silicane hydroxide and mass percent concentration are that 15% dilute hydrochloric acid solution reacts in hydrolytic reaction pot with mass percentage content, hydrolysis temperature is controlled at about 20 ℃, reaction times is 4 hours, the volume ratio of dimethyl silicane hydroxide and dilute hydrochloric acid is 1:8, and the product of reaction is hydrogenchloride, tetramethyl-dihydro sily oxide and a small amount of oligopolymer.After reaction finished, product filtered, and removes a small amount of solid impurity.
(2) product after the filtration enters the phase separator standing demix.Lower floor is the hydrochloric acid water after the layering, and the upper strata is siloxanes crude product phase, lower floor's hydrochloric acid water is separated in phase separator, but the hydrolysis stopper is done in reuse after the waste hydrochloric acid dilution.
The tetramethyl-dihydro sily oxide crude product that (3) will obtain from phase separator is repeatedly washed in washing kettle, until the crude product system is neutral.
(4) will be neutral tetramethyl-dihydro sily oxide crude product passes into and carries out rectifying in the rectifying tower, the rectifying condition is with embodiment 2, obtain the tetramethyl-dihydro sily oxide that purity is about 99.7%, chloride ion content is about 5ppm, a small amount of low-boiling-point substance and oligopolymer then reuse are done other products.The final tetramethyl-dihydro sily oxide yield that calculates is about 87%.
Embodiment 4
(1) be that 97% dimethyl silicane hydroxide and mass percent concentration are that 15% dilute hydrochloric acid solution reacts in hydrolytic reaction pot with mass percentage content, hydrolysis temperature is controlled at about 25 ℃, reaction times is 6 hours, the volume ratio of dimethyl silicane hydroxide and dilute hydrochloric acid is 1:5, the product of reaction is hydrogenchloride, tetramethyl-dihydro sily oxide and a small amount of oligopolymer, after reaction finished, product filtered, and removes a small amount of solid impurity.
(2) product after the filtration enters the phase separator standing demix.Lower floor is the hydrochloric acid water after the layering, and the upper strata is siloxanes crude product phase, lower floor's hydrochloric acid water is separated in phase separator, but the hydrolysis stopper is done in reuse after the waste hydrochloric acid dilution.
The tetramethyl-dihydro sily oxide crude product that (3) will obtain from phase separator is repeatedly washed in washing kettle, until the crude product system is neutral.
(4) will be neutral tetramethyl-dihydro sily oxide crude product passes into and carries out rectifying in the rectifying tower, the rectifying condition is with embodiment 2, obtain the tetramethyl-dihydro sily oxide that purity is about 99.9%, chloride ion content is about 6ppm, a small amount of low-boiling-point substance and oligopolymer then reuse are done other products.The final tetramethyl-dihydro sily oxide yield that calculates is about 85%.

Claims (7)

1. a device for preparing tetramethyl-dihydro sily oxide is characterized in that, comprising:
Hydrolytic reaction pot with dilute hydrochloric acid opening for feed and dimethyl silicane hydroxide opening for feed;
The phase-separating device that opening for feed is communicated with the discharge port of hydrolytic reaction pot;
Be located at the first control valve on the pipeline between the opening for feed of the discharge port of hydrolytic reaction pot and phase-separating device;
The washing kettle that opening for feed is communicated with the organic phase discharge port of phase-separating device, on the washing kettle with the washing water opening for feed;
The rectifier unit that opening for feed is communicated with the discharge port of washing kettle.
2. the device of preparation tetramethyl-dihydro sily oxide according to claim 1 is characterized in that, the pipeline between the discharge port of described the first control valve and the opening for feed of phase-separating device is provided with strainer.
3. the device of preparation tetramethyl-dihydro sily oxide according to claim 1 is characterized in that, described phase-separating device is the liquid-liquid phase separation device, and the inorganic phase discharge port of liquid-liquid phase separation device is communicated with the dilute hydrochloric acid opening for feed of hydrolytic reaction pot.
4. the device of preparation tetramethyl-dihydro sily oxide according to claim 1, it is characterized in that, pipeline between the dilute hydrochloric acid feeding mouth of described hydrolytic reaction pot and the inorganic phase discharge port of liquid-liquid phase separation device is provided with the dilute hydrochloric acid storage tank, and the pipeline between the dilute hydrochloric acid feeding mouth of the discharge port of this dilute hydrochloric acid storage tank and hydrolytic reaction pot is provided with the second control valve.
5. the device of preparation tetramethyl-dihydro sily oxide according to claim 1, it is characterized in that, also comprise the dimethyl silicane hydroxide storage tank, the dimethyl silicane hydroxide opening for feed of described hydrolytic reaction pot is communicated with the discharge port of this dimethyl silicane hydroxide storage tank, and pipeline between the two is provided with the 3rd control valve.
6. the device of preparation tetramethyl-dihydro sily oxide according to claim 1, it is characterized in that, also comprise the deionized water hold-up vessel, the washing water opening for feed of described washing kettle is communicated with the discharge port of this deionized water storage tank, and pipeline between the two is provided with the 4th control valve.
7. the device of preparation tetramethyl-dihydro sily oxide according to claim 1 is characterized in that, described rectifier unit is plate distillation column.
CN 201220371302 2012-07-30 2012-07-30 Device for preparing tetramethyldihydrodisiloxane Expired - Lifetime CN202705272U (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201220371302 CN202705272U (en) 2012-07-30 2012-07-30 Device for preparing tetramethyldihydrodisiloxane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201220371302 CN202705272U (en) 2012-07-30 2012-07-30 Device for preparing tetramethyldihydrodisiloxane

Publications (1)

Publication Number Publication Date
CN202705272U true CN202705272U (en) 2013-01-30

Family

ID=47585593

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201220371302 Expired - Lifetime CN202705272U (en) 2012-07-30 2012-07-30 Device for preparing tetramethyldihydrodisiloxane

Country Status (1)

Country Link
CN (1) CN202705272U (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563753A (en) * 2019-08-05 2019-12-13 潜江宜生新材料有限公司 Photochlorination system of methyl trichlorosilane
CN115521331A (en) * 2022-10-14 2022-12-27 唐山三友化工股份有限公司 Continuous efficient hydrolysis method and device for dimethylchlorosilane

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110563753A (en) * 2019-08-05 2019-12-13 潜江宜生新材料有限公司 Photochlorination system of methyl trichlorosilane
CN110563753B (en) * 2019-08-05 2022-04-26 潜江宜生新材料有限公司 Photochlorination system of methyl trichlorosilane
CN115521331A (en) * 2022-10-14 2022-12-27 唐山三友化工股份有限公司 Continuous efficient hydrolysis method and device for dimethylchlorosilane

Similar Documents

Publication Publication Date Title
CN102757458B (en) Method and device for preparing tetramethyldihydrodisiloxane
CN101875726B (en) Method for preparing polysiloxane by hydrolyzing dimethyl dichlorosilane
CN106866954B (en) A kind of cation polyether reverse-phase emulsifier and preparation method thereof
EP2491071B1 (en) Process for preparing organopolysiloxanes
CN104530967A (en) Reactive organosilicon waterproofing agent as well as preparation method and application thereof
CN104151585B (en) A kind of preparation method of the calcium carbonate-filled polyurethane infiltrating and vaporizing membrane of dewatering nano
CN106397368A (en) Fatty alcohol-polyoxyethylene ether glycidyl ether and preparation method thereof
CN202705272U (en) Device for preparing tetramethyldihydrodisiloxane
CN105061767A (en) Dimethyl dichlorosilance hydrolysis process and device
CN101058585B (en) Safe separation method for increasing yield of methyl phenyl dialkoxy silicane
CN104945428A (en) Method for preparing dimethyl dichlorosilane
CN105111440B (en) A kind of continuous environment-friendly preparation process of high-temperature resistant coating methyl phenyl silicone resin
CN104558611B (en) A kind of MDTQ silicones and its preparation method and application
CN102492144A (en) Saturated acid hydrolysis technology of alkylchlorosilane
CN110981902A (en) Preparation method of modified monomethyl-tributyl ketoxime silane
CN102516599A (en) Method for synthesizing mixed ketoxime cross-linking agent
CN103319519A (en) Method for producing hexamethyldisiloxane by utilization of organosilicon azeotrope
CN106317095A (en) Hydrolysis technology and device for concentrated hydrochloric acid
CN105315139B (en) A kind of processing method of ketoxime type silane by-products ketoxime salt
CN101503422B (en) Method for preparing methyl phenyl ring siloxane mixture
CN112358616A (en) Process method for removing residual chlorine at terminal hydroxyl of polysiloxane hydrolysate
CN102993226A (en) Method for preparing phenyl dimethylchlorosilane
CN101735258B (en) Method for preparing micromolecular hydroxyl silicone oil
CN102250133A (en) Method for preparing dimethyl dichlorosilane by using disproportionation method
CN1249127C (en) Process for preparing high boiling silicone oil by using organic high boiling point matter

Legal Events

Date Code Title Description
C14 Grant of patent or utility model
GR01 Patent grant
CX01 Expiry of patent term
CX01 Expiry of patent term

Granted publication date: 20130130