CN106928458A - A kind of method that utilization high-boiling components cracking raffinate prepares high boiling point silicon oil - Google Patents
A kind of method that utilization high-boiling components cracking raffinate prepares high boiling point silicon oil Download PDFInfo
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- CN106928458A CN106928458A CN201710099469.9A CN201710099469A CN106928458A CN 106928458 A CN106928458 A CN 106928458A CN 201710099469 A CN201710099469 A CN 201710099469A CN 106928458 A CN106928458 A CN 106928458A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
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Abstract
The present invention relates to the method that a kind of utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, its step is as follows：(1) height boiling raffinate is obtained after the dimethyldichlorosilane in the product after cracking organosilicon high-boiling product is separated；(2) add trim,ethylchlorosilane as end-capping reagent in height boiling raffinate, obtain height boiling and mix residual night, the addition of trim,ethylchlorosilane is that every 1000ML adds 3-30g trim,ethylchlorosilanes in height boiling raffinate；(3) be hydrolyzed reaction in height boiling being mixed into residual night and saturation hydrochloric acid solution addition hydrolysis device, generation high boiling point silicon oil, the hydrogen chloride gas generated in hydrolytic process can not be dissolved in saturation hydrochloric acid solution, but directly extracted out through hydrolysis device, chloromethanes synthetic reaction is directly used in after scrubbed, the height boiling raffinate that will be produced after cracking organosilicon high-boiling product continues on for producing high boiling point silicon oil, improves business efficiency, efficiency has been saved, the outer row of low-grade hydrochloric acid has been significantly reduced.
Description
Technical field
The present invention relates to a kind of preparation method of high boiling point silicon oil, and in particular to one kind is prepared high using high-boiling components cracking raffinate
The method of boiling point silicon oil.
Background technology
Organosilicon high-boiling product refers to the higher boiling silane mixture of generation in methyl chlorosilane monomer building-up process, accounts for mixing
The 5% of monomer composition is closed, high-boiling components can not be made into useful organopolysiloxane, existing organosilicon with simple method
The processing method of high-boiling components is divided into two methods of hydrogen chloride catalytic pyrolysis and high-pressure catalytic cracking, two kinds of high-boiling components of cleavage method
Conversion per pass is more than 80%.But, even so, cracking raffinate is still present after high-boiling components cracking, this part of thing
Matter belongs to dangerous waste, it is impossible to be used well, there is certain waste；
Accordingly, it would be desirable to high-boiling components cracking raffinate to be prepared into a kind of method the high boiling point silicon oil of high-quality, the change of high boiling point silicon oil
Scientific name claims to be methylmethoxysilane mixing EVA, is faint yellow or light brown oil liquid, with heat resistance, electric insulation
Property, weatherability, hydrophobicity, physiological inertia and less surface tension, relatively low viscosity-temperature coefficient, resistance to compression higher, resistance to spoke
The characteristics of, it is applied to be carried out for methyl-silicone oil the preparation of fluid sealant.
The content of the invention
The present invention proposes one kind and uses high-boiling components cracking raffinate to prepare height using saturation acid-hydrolysis method regarding to the issue above
The method of boiling point silicon oil, the height boiling raffinate that will be produced after cracking organosilicon high-boiling product continue on for produce high boiling point silicon oil, improve through
Ji efficiency, has saved efficiency, reduces cost, significantly reduces the outer row of low-grade hydrochloric acid.
Specific technical scheme is as follows：
A kind of method that utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, its step is as follows：
(1) height boiling raffinate is obtained after the dimethyldichlorosilane in the product after cracking organosilicon high-boiling product is separated；
(2) add trim,ethylchlorosilane as end-capping reagent in height boiling raffinate, obtain height boiling and mix residual night, trimethylchloro-silicane
The addition of alkane is that every 1000ML adds 3-30g trim,ethylchlorosilanes in height boiling raffinate；
(3) be hydrolyzed reaction in height boiling being mixed into residual night and saturation hydrochloric acid solution addition hydrolysis device, generates high boiling-point silicon
Oil, the hydrogen chloride gas generated in hydrolytic process can not be dissolved in saturation hydrochloric acid solution, but directly be extracted out through hydrolysis device, pass through
Chloromethanes synthetic reaction is directly used in after washing, purifying；Kinematic viscosity≤50mm of the high boiling point silicon oil of production at 25 DEG C2/ s,
Density at 25 DEG C is 0.80-0.97g/mL.
The method that a kind of above-mentioned utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, wherein, the hydrolysis device includes height
The residual night storage tank of boiling mixing, circulating pump, saturation concentrated hydrochloric acid storage tank, the first packed tower, the second packed tower and knockout drum, the first packed tower
It is provided with first charging aperture and the first discharging opening, first charging aperture is located at the first discharging opening lower section, the second packed tower is provided with the
Two charging apertures and the second discharging opening, the second discharging opening are located at the top of second charging aperture, and knockout drum is provided with the 3rd charging aperture, the
Three discharging openings and the 4th discharging opening, the 4th discharging opening are located at the 3rd discharging opening top；First discharging opening passes through with second charging aperture
First pipeline is connected, and the second discharging opening is connected with the 3rd charging aperture by second pipe, and the 3rd discharging opening and first feeds
Mouth is connected by the 3rd pipeline, forms circulation line, and circulating pump is arranged on the 3rd pipeline, and height boiling mixes residual night storage tank and satisfies
It is connected with the 3rd pipeline by the 4th pipeline and the 5th pipeline respectively with concentrated hydrochloric acid storage tank, it is unidirectional that the 4th pipeline is provided with first
Valve, the 5th pipeline is provided with the second check valve, and the second packed tower top is provided with gas outlet, and gas outlet is provided with the 6th pipeline, the
Six pipelines are provided with the 3rd check valve, and the 4th discharging opening is provided with the 7th pipeline, and the 7th pipeline is provided with the 4th check valve.
The method that a kind of above-mentioned utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, wherein, first packed tower includes
The second pressing plate, the first pressing plate, the first filler, the first pressing plate and second are sequentially provided with from top to bottom in first tower body, the first tower body
Pressing plate, first pressing plate includes the first support ring of cirque structure and being fixed between the first support ring for being parallel to each other
Support bar, second pressing plate includes the second supporting plate of circular configuration, and the second supporting plate is provided with some second through holes.
The method that a kind of above-mentioned utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, wherein, second packed tower includes
Demister, the second pressing plate, the first pressing plate, the second filler, the first pressing plate are sequentially provided with from top to bottom in second tower body, the second tower body
With the second pressing plate.
The method that a kind of above-mentioned utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, wherein, the volume of second filler
It is the 2/3 of the first packing volume.
The method that a kind of above-mentioned utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, wherein, first pressing plate is with steel
Material, outside is provided with one layer of polytetrafluoroethylene floor；Second pressing plate is made up with polytetrafluoroethylene (PTFE) of material.
Beneficial effects of the present invention are：
The height boiling raffinate that the present invention will be produced after cracking organosilicon high-boiling product continues on for producing high boiling point silicon oil, for pin
Sell, reduce percent defective, improve business efficiency, saved efficiency, reduce cost, significantly reduce the outer of low-grade hydrochloric acid
Row.
Brief description of the drawings
Fig. 1 is hydrolysis device structure chart of the present invention.
Fig. 2 is the first pressure plate structure figure of the invention.
Fig. 3 is the second pressure plate structure figure of the invention.
Fig. 4 is support bar sectional view of the present invention.
Fig. 5 is the first pressing plate of the invention and the second pressing plate overlapping schematic diagram.
Specific embodiment
To make technical scheme become apparent from clearly, the present invention is described further below in conjunction with the accompanying drawings,
Any technical characteristic to technical solution of the present invention carries out the scheme that equivalencing and conventional reasoning draw and each falls within guarantor of the present invention
Shield scope.
Reference
Height boiling mix residual night storage tank 1, circulating pump 2, saturation concentrated hydrochloric acid storage tank 3, the first packed tower 4, the second packed tower 5, point
Discharged from tank 6, first charging aperture 7, the first discharging opening 8, second charging aperture 9, the second discharging opening 10, the 3rd charging aperture the 11, the 3rd
The 12, the 4th discharging opening 13 of mouth, the first pipeline 14, second pipe 15, the 3rd pipeline 16, the 4th pipeline 17, the 5th pipeline 18, first
Check valve 19, the second check valve 20, gas outlet 21, the 6th pipeline 22, the 3rd check valve 23, the 7th pipeline 24, the 4th check valve
25th, the first tower body 26, the second pressing plate 27, the first pressing plate 28, the first filler 29, the first support ring 32, support bar 33, second are supported
Plate 34, the second through hole 35, the second tower body 36, demister 37, the second filler 38, permeable hole group 39.
, it is necessary to use hydrolysis device when the present invention prepares high boiling point silicon oil using high-boiling components cracking raffinate, the hydrolysis device,
Mix residual night storage tank 1, circulating pump 2, saturation concentrated hydrochloric acid storage tank 3, the first packed tower 4, the second packed tower 5 and knockout drum including height boiling
6, the first packed tower is provided with the discharging opening 8 of first charging aperture 7 and first, and first charging aperture is located at the first discharging opening lower section, second
Packed tower is provided with the discharging opening 10 of second charging aperture 9 and second, and the second discharging opening is located at the top of second charging aperture, on knockout drum
The 3rd charging aperture 11, the 3rd discharging opening 12 and the 4th discharging opening 13 are provided with, the 4th discharging opening is located at the 3rd discharging opening top；First
Discharging opening is connected with second charging aperture by the first pipeline 14, and the second discharging opening passes through the phase of second pipe 15 with the 3rd charging aperture
Connection, the 3rd discharging opening is connected by the 3rd pipeline 16 with first charging aperture, forms circulation line, and circulating pump is arranged on the 3rd
On pipeline, height boiling mixes residual night storage tank and saturation concentrated hydrochloric acid storage tank respectively by the 4th pipeline 17 and the 5th pipeline 18 and the 3rd pipe
Road is connected, and the 4th pipeline is provided with the first check valve 19, and the 5th pipeline is provided with the second check valve 20, the second packed tower top
Gas outlet 21 is provided with, gas outlet is provided with the 6th pipeline 22, and the 6th pipeline is provided with the 3rd check valve 23, is set on the 4th discharging opening
There is the 7th pipeline 24, the 7th pipeline is provided with the 4th check valve 25.
First packed tower includes the first tower body 26, is sequentially provided with the second pressing plate 27, the in the first tower body from top to bottom
One pressing plate 28, the first filler 29, the first pressing plate and the second pressing plate, first pressing plate include the first support ring of cirque structure
32 and the support bar 33 being fixed between the first support ring that is parallel to each other, second pressing plate includes second of circular configuration
Fagging 34, the second supporting plate is provided with some second through holes 35.
Second packed tower includes being sequentially provided with demister 37, second from top to bottom in the second tower body 36, the second tower body
Pressing plate, the first pressing plate, the second filler 38, the first pressing plate and the second pressing plate；The volume of second filler is the first packing volume
2/3, with steel as material, outside is provided with one layer of polytetrafluoroethylene floor to first pressing plate；Second pressing plate is with polytetrafluoroethyl-ne
Alkene is made up of material.
Further, the cross sectional shape of the support bar of first pressing plate is isosceles trapezoidal structure, two neighboring support bar
Between spacing be h1；Second pressing plate forms some permeable hole groups by the arrangement in alignment of some second through holes
39, the second through hole between two neighboring permeable hole group is staggered, and the distance between two neighboring permeable hole group is d2, second
The aperture of through hole is d1, h1=3*d1, d2=d1；First pressing plate is superimposed with each other with the second pressing plate, support bar and permeable hole
Group is mutually perpendicular to intersect.
Further, the width that support bar section is in the upper bottom of isosceles trapezoid is h2, and support bar section is in isosceles ladder
The width of the bottom of shape is in the upper of isosceles trapezoid for the support bar section of h3, h2=0.8*d1, h3=1.5*d1, the first pressing plate
Bottom one side is in contact with the second pressing plate, and the height of the support bar is identical with the thickness of the first support ring.
A kind of method that utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, its step is as follows：
(1) height boiling is obtained after the dimethyldichlorosilane in the product after cracking organosilicon high-boiling product is totally separated residual
Liquid, wherein, the composition of organosilicon high-boiling product is shown in Table 1, and the product composition after cracking is shown in Table 2；
(2) add trim,ethylchlorosilane as end-capping reagent in height boiling raffinate, obtain height boiling and mix residual night, trimethylchloro-silicane
The addition of alkane is that every 1000ML adds 3-30g trim,ethylchlorosilanes in height boiling raffinate；
(3) by height boiling mix residual night mix with saturation hydrochloric acid solution after pass through by the 3rd pipeline enter the first packed tower in,
Be hydrolyzed reaction in first packed tower, after hydrolysis again via the first pipeline into being hydrolyzed in the second packed tower and
Reaction is separated, isolated hydrogen chloride gas are discharged from the 5th pipeline, and isolated head product enters by the second discharging opening
Enter in knockout drum, head product forms the hierarchy of bottom hydrochloric acid, top end-product after stabilization in knockout drum, and high boiling point silicon oil is certainly
4th discharging opening is discharged through the 7th pipeline, and hydrochloric acid enters in the 3rd pipeline from the 3rd discharging opening and continues circular response, height boiling mixing
Residual night storage tank and saturation concentrated hydrochloric acid storage tank are constantly to adding new dimethyldichlorosilane and saturation concentrated hydrochloric acid in circulation line
Circulated with maintenance reaction and occurred, the hydrogen chloride gas generated in hydrolytic process can not be dissolved in saturation hydrochloric acid solution, but through hydrolysis
Device is directly extracted out, it is scrubbed after be directly used in chloromethanes synthetic reaction.
Table 1：The constituent of organosilicon high-boiling product.
Table 2：Product constituent after cracking.
| Sequence number | Reactant | Content (wt%) |
| 1 | MeSiCl3 | 3.8 |
| 2 | Me2SiCl2 | 64.3 |
| 3 | Me3SiCl | 0 |
| 4 | HMeSiCl2 | 9.9 |
| 5 | HMe2SiCl | 15.6 |
| 6 | H2MeSiCl | 2.4 |
| 7 | HSiCl3 | 0 |
| 8 | Impurity | Surplus |
Wherein, Me nails base (- CH3)。
Table 3：The testing result of the high boiling point silicon oil of production.
| Project | Index request |
| Outward appearance | Light yellow or brown oil liquid |
| Kinematic viscosity (mm2/s)25℃ | ≤50 |
| 25 DEG C of density (g/mL) | 0.80‐0.97 |
The height boiling raffinate that the present invention will be produced after cracking organosilicon high-boiling product continues on for producing high boiling point silicon oil, for pin
Sell, reduce percent defective, improve business efficiency, saved efficiency, reduce cost.
At the same time, the present invention uses two packed towers, is reacted in the first packed tower, and the second packed tower is divided
From, the impurity content in hydrogen chloride is reduced, the yield of hydrolysate is improve, make reaction more complete, energy consumption is reduced, reduce
Cost, need to such as increase production capacity, then can not completely interfere with reaction directly to be realized by way of increasing packed tower volume
Efficiency, so as to effectively realize the purpose of lifting production capacity.
Claims (5)
1. a kind of method that utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, it is characterized by, its step is as follows：
(1) height boiling raffinate is obtained after the dimethyldichlorosilane in the product after cracking organosilicon high-boiling product is separated；
(2) add trim,ethylchlorosilane as end-capping reagent in height boiling raffinate, obtain height boiling and mix residual night, trim,ethylchlorosilane
Addition is that every 1000ML adds 3-30g trim,ethylchlorosilanes in height boiling raffinate；
(3) be hydrolyzed reaction in height boiling being mixed into residual night and saturation hydrochloric acid solution addition hydrolysis device, generates high boiling point silicon oil, water
The hydrogen chloride gas generated in solution preocess can not be dissolved in saturation hydrochloric acid solution, but directly be extracted out through hydrolysis device, scrubbed
Chloromethanes synthetic reaction is directly used in after purification；Kinematic viscosity≤50mm of the high boiling point silicon oil of production at 25 DEG C2/ s, at 25 DEG C
Under density be 0.80-0.97g/mL.
2. the method that a kind of utilization high-boiling components cracking raffinate as claimed in claim 1 prepares high boiling point silicon oil, it is characterized by, it is described
Hydrolysis device includes that height boiling mixes residual night storage tank, circulating pump, saturation concentrated hydrochloric acid storage tank, the first packed tower, the second packed tower and divides
From tank, the first packed tower is provided with first charging aperture and the first discharging opening, and first charging aperture is located at the first discharging opening lower section, second
Packed tower is provided with second charging aperture and the second discharging opening, and the second discharging opening is located at the top of second charging aperture, is set on knockout drum
There are the 3rd charging aperture, the 3rd discharging opening and the 4th discharging opening, the 4th discharging opening is located at the 3rd discharging opening top；First discharging opening with
Second charging aperture is connected by the first pipeline, and the second discharging opening is connected with the 3rd charging aperture by second pipe, and the 3rd goes out
Material mouth is connected by the 3rd pipeline with first charging aperture, forms circulation line, and circulating pump is arranged on the 3rd pipeline, and height boiling is mixed
Close residual night storage tank and saturation concentrated hydrochloric acid storage tank is connected by the 4th pipeline and the 5th pipeline with the 3rd pipeline respectively, the 4th pipeline
The first check valve is provided with, the 5th pipeline is provided with the second check valve, and the second packed tower top is provided with gas outlet, is set on gas outlet
There is the 6th pipeline, the 6th pipeline is provided with the 3rd check valve, and the 4th discharging opening is provided with the 7th pipeline, and the 7th pipeline is provided with
Four check valves.
The method that a kind of above-mentioned utilization high-boiling components cracking raffinate prepares high boiling point silicon oil, wherein, first packed tower includes first
The second pressing plate, the first pressing plate, the first filler, the first pressing plate and the second pressing plate are sequentially provided with from top to bottom in tower body, the first tower body,
The support being fixed between the first support ring that first pressing plate includes the first support ring of cirque structure and is parallel to each other
Bar, second pressing plate includes the second supporting plate of circular configuration, and the second supporting plate is provided with some second through holes.
3. the method that a kind of utilization high-boiling components cracking raffinate as claimed in claim 2 prepares high boiling point silicon oil, it is characterized by, it is described
Second packed tower includes the second tower body, is sequentially provided with demister, the second pressing plate, the first pressing plate, the in the second tower body from top to bottom
Two fillers, the first pressing plate and the second pressing plate.
4. the method that a kind of utilization high-boiling components cracking raffinate as claimed in claim 2 prepares high boiling point silicon oil, it is characterized by, it is described
The volume of the second filler is the 2/3 of the first packing volume.
5. the method that a kind of utilization high-boiling components cracking raffinate as claimed in claim 2 prepares high boiling point silicon oil, it is characterized by, it is described
With steel as material, outside is provided with one layer of polytetrafluoroethylene floor to first pressing plate；Second pressing plate is with polytetrafluoroethylene (PTFE) as material system
Into.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142975A (en) * | 2020-09-16 | 2020-12-29 | 湖北兴瑞硅材料有限公司 | Method for comprehensively utilizing organic silicon byproduct high-boiling residues |
| CN113842870A (en) * | 2021-10-29 | 2021-12-28 | 新疆晶硕新材料有限公司 | Device and method for continuously preparing high-boiling silicone oil |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061766A (en) * | 2015-09-16 | 2015-11-18 | 浙江新安化工集团股份有限公司 | Treatment device and method for organic silicon waste liquor |
| CN106188545A (en) * | 2016-08-30 | 2016-12-07 | 浙江中天氟硅材料有限公司 | Utilize the method that organosilicon high-boiling product prepares inertia high boiling point silicon oil |
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2017
- 2017-02-23 CN CN201710099469.9A patent/CN106928458A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105061766A (en) * | 2015-09-16 | 2015-11-18 | 浙江新安化工集团股份有限公司 | Treatment device and method for organic silicon waste liquor |
| CN106188545A (en) * | 2016-08-30 | 2016-12-07 | 浙江中天氟硅材料有限公司 | Utilize the method that organosilicon high-boiling product prepares inertia high boiling point silicon oil |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112142975A (en) * | 2020-09-16 | 2020-12-29 | 湖北兴瑞硅材料有限公司 | Method for comprehensively utilizing organic silicon byproduct high-boiling residues |
| CN112142975B (en) * | 2020-09-16 | 2022-08-05 | 湖北兴瑞硅材料有限公司 | Method for comprehensively utilizing organic silicon byproduct high-boiling residues |
| CN115490862A (en) * | 2020-09-16 | 2022-12-20 | 湖北兴瑞硅材料有限公司 | Comprehensive utilization method of organic silicon byproduct high-boiling residues |
| CN115490862B (en) * | 2020-09-16 | 2023-07-11 | 湖北兴瑞硅材料有限公司 | Comprehensive utilization method of organic silicon byproduct high-boiling-point substances |
| CN113842870A (en) * | 2021-10-29 | 2021-12-28 | 新疆晶硕新材料有限公司 | Device and method for continuously preparing high-boiling silicone oil |
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Application publication date: 20170707 |