CN103450249B - The process for purification of methyl cyclosiloxane - Google Patents
The process for purification of methyl cyclosiloxane Download PDFInfo
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- CN103450249B CN103450249B CN201310347812.9A CN201310347812A CN103450249B CN 103450249 B CN103450249 B CN 103450249B CN 201310347812 A CN201310347812 A CN 201310347812A CN 103450249 B CN103450249 B CN 103450249B
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- methyl cyclosiloxane
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- filter cake
- cyclosiloxane
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Abstract
The process for purification of a kind of methyl cyclosiloxane, relates to technical field of chemical products, by refined methyl cyclosiloxane, activated carbon, flocculant, industrial soda in the ratio mixing and stirring of 100:12.5:1:1, forms adjuvant mixture stand-by；Forming filter cake in adjuvant mixture is driven into pressure filter by gear pump, this filter cake is for filtering thick methyl cyclosiloxane to be processed；Filtered by filter cake in the thick methyl cyclosiloxane that obtains of organic silicon scrap cracking is squeezed into pressure filter successively, the effect of filtration be thick methyl cyclosiloxane is neutralized, remove impurity, decolouring；Filtration obtains fine work methyl cyclosiloxane after completing, can be directly used for preparing organosilicon downstream product, it is possible to use as adjuvant.Preparation method of the present invention is simple, it is simple to practical operation, does not has the generation of waste water, garbage, will not damage environment, and energy loss is few, and finished product purity is high, has extraordinary practice meaning.
Description
Technical field
The present invention relates to technical field of chemical products, be specifically related to a kind of use washing, neutralize, the process technique that precipitates essence
The method of methyl cyclosiloxane processed.
Background technology
Methyl cyclosiloxane is to prepare the intermediate of the polysiloxane such as silicone rubber, silicone oil, can be further processed into resistance to
Multiple silicone rubber that high/low temperature, good insulation preformance, weather-resistant, resistance to ozone, radiation resistance are good, silicone oil.
In prior art, the preparation of methyl cyclosiloxane uses the silicone rubber scrapped, and material scrapped by silastometer or other organosilicon
For raw material, with sulphuric acid and 12 chain phenylbenzimidazole sulfonic acids be catalyst under the high temperature conditions, convert feedstock into methyl cyclosiloxane thick
Goods.And be that neutralization reset under the high temperature conditions by catalyst with potassium hydroxide, then filter with activated carbon adsorption, it is thus achieved that methyl ring
Siloxane and refining product.It is that catalyst can be made into silicon under certain condition by methyl cyclosiloxane highly finished product Tetramethylammonium hydroxide
Oil, the product such as silicone rubber, then add activated carbon adsorption and filter standby storehouse.Wherein the subtractive process of methyl cyclosiloxane need to be at high temperature bar
Carrying out under part, careless manipulation easily causes tactile glue (reactor, condenser blocks up glue) and produces high pressure, even spontaneous combustion；And emptying bleeds off pressure
Time will produce a certain amount of foul smell.Refining in terms of 1000kg methyl cyclosiloxane by every batch, this rearrangement neutralizes technique time-consuming seven
Hour, add activated carbon adsorption and filter four hours, power consumption 1300 degree, about 300 yuan/still of catalyst, about 150 yuan/still of activated carbon, essence
Process processed is the longest, power consumption is high, and safety coefficient is low, has certain pollution to environment, and material loss (is about lost greatly
3%), the actual 970kg that obtains, relatively costly.
Additionally, the refined employing negative-pressure operation of a kind of mixed methyl cyclosiloxane.Mixed methyl cyclosiloxane is through pre-
Entering de-low tower after the preheating of hot device, reboiler leads to middle pressure steam and heats tower, and overhead condenser leads to hot water condensation.In vacuum system
Making under negative pressure, the material being condensed enters return tank, carries out total reflux operation through reflux pump, determines that reflux pump exports thing through analyzing
After in material and kettle material, each constituent content is qualified, the material extraction in return tank is to packing jar, is more extremely wrapped by packaging pump extraction
Pack between dress.Meanwhile, the mixed methyl cyclosiloxane after tower reactor extraction is de-light is to finishing column, for further processing and smart
System.
It is 75 ± 5 DEG C at reflux temperature, in the case of vacuum is 0.069MPa, still has part methyl cyclosiloxane (light
Component, particularly hexamethyl cyclotrisiloxane), can be brought in vacuum system, cause vacuum pipeline to block, have part six simultaneously
Methyl cyclotrisiloxane enters in vacuum water tank, because its density is more than water, can sink to water tank bottom, entering of blocking water ring vacuum pump
The mouth of a river, makes vacuum pump set stop jumping or damages water ring vacuum pump.So be easily caused system must parking process, expend a large amount of manpower and
Time carries out dredging cleaning to vacuum system, affects production efficiency, and increases the labor intensity carrying out operator.
Chinese patent CN201676545U discloses a kind of mixed methyl siloxane constant pressure light-eliminating device, and it includes preheating
Device, lightness-removing column, reboiler, extraction ball valve, finished product feed pump etc., its atmospheric operation avoids negative pressure to refine the vacuum breast blocking caused
Problem, improve production efficiency, reduce cost and labor intensity.But this refining plant and process for purification are complex, and set
Standby investment is big, and refining effect is poor.
Summary of the invention
The technical problem to be solved is to provide that a kind of simple and safe environmental protection of technique, response time be short, cost
The process for purification of the methyl cyclosiloxane that low-yield is high and purified product purity is high.
The technical problem to be solved realizes by the following technical solutions:
A kind of process for purification of methyl cyclosiloxane, including following methods step,
1) first refined methyl cyclosiloxane (fine work), activated carbon, flocculant, industrial soda are pressed 100:12.5:1:1's
Ratio mixing and stirring, forms adjuvant mixture stand-by；
2) forming filter cake in adjuvant mixture being driven into pressure filter by gear pump, this filter cake is to be processed for filtering
Thick methyl cyclosiloxane；
3) carried out by filter cake in the thick methyl cyclosiloxane that organic silicon scrap cracking obtains being squeezed into pressure filter successively
Filter, the effect of filtration be thick methyl cyclosiloxane is neutralized, remove impurity, decolouring；
4) obtain fine work methyl cyclosiloxane after having filtered, can be directly used for preparing organosilicon downstream product, it is also possible to
Use as adjuvant in step 1).
When filter cake occurs filtering slow in pressure filter, being opened by pressure filter, filter cake shovel is fallen, the filter cake after shovel falls can be mixed
Entering in organic silicon scrap and crack, again make filter cake, under normal circumstances, Primary batching system may filter that 3-5 ton thick methyl ring silicon
Oxygen alkane.
Described pressure filter is a 10m2Plate and frame type filter-press.
Described gear pump is the gear pump of 1.5 kilowatts.
The invention has the beneficial effects as follows: preparation method of the present invention is simple, it is simple to practical operation there is no waste water, garbage
Producing, will not damage environment, energy loss is few, and finished product purity is high, has extraordinary practice meaning.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and be easy to understand with effect, below knot
Close specific embodiment, the present invention is expanded on further.
Embodiment 1
One, equipment a: 10m2 Plate and frame type filter-press
One 1.5 kilowatts of gear pump.
Two, adjuvant: 25kg activated carbon adds 2kg flocculant and adds 2kg industrial soda, stirs；
Three, technique: above-mentioned adjuvant is poured in 200kg methyl cyclosiloxane (fine work), stir, beaten by gear pump
Form filter cake in entering pressure filter, the thick methyl cyclosiloxane (3 tons) that organic silicon scrap cracking obtains is squeezed in pressure filter successively
Filter, can be by thick methyl cyclosiloxane neutralization, decontamination, decolouring, finished product directly does organosilicon downstream product.
(filter slowly) after reaching certain sword in pressure filter, pressure filter is opened, filter cake shovel is fallen (can mix in useless silica gel
Crack), again make filter cake, the general filter thick methyl cyclosiloxane of 3-5 ton (crude oil) tears sheet frame shovel filter cake open.
Embodiment 2
One, equipment a: 10m2 Plate and frame type filter-press
One 1.5 kilowatts of gear pump.
Two, adjuvant: 200kg methyl cyclosiloxane (fine work) adds 25kg activated carbon and adds 2kg flocculant and add 2kg industrial soda, stirs
Mix uniformly, form adjuvant mixture stand-by；
Three, technique:
1) forming filter cake in adjuvant mixture being driven into pressure filter by gear pump, this filter cake is to be processed for filtering
Thick methyl cyclosiloxane；
2) carried out by filter cake in the thick methyl cyclosiloxane that organic silicon scrap cracking obtains being squeezed into pressure filter successively
Filter, the effect of filtration be thick methyl cyclosiloxane is neutralized, remove impurity, decolouring；
3) obtain fine work methyl cyclosiloxane after having filtered, can be directly used for preparing organosilicon downstream product, it is also possible to
Use as adjuvant in step 1).
When filter cake occurs filtering slow in pressure filter, being opened by pressure filter, filter cake shovel is fallen, the filter cake after shovel falls can be mixed
Entering in organic silicon scrap and crack, again make filter cake, under normal circumstances, Primary batching system may filter that 3-5 ton thick methyl ring silicon
Oxygen alkane.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.The technology of the industry
Personnel, it should be appreciated that the present invention is not restricted to the described embodiments, simply illustrating this described in above-described embodiment and description
The principle of invention, without departing from the spirit and scope of the present invention, the present invention also has various changes and modifications, and these become
Change and improvement both falls within scope of the claimed invention.Claimed scope by appending claims and
Equivalent defines.
Claims (4)
1. the process for purification of a methyl cyclosiloxane, it is characterised in that: include following methods step,
1) refined methyl cyclosiloxane, activated carbon, flocculant, industrial soda is equal in the ratio mix and blend of 100:12.5:1:1
Even, form adjuvant mixture stand-by；
2) forming filter cake in adjuvant mixture being driven into pressure filter by gear pump, this filter cake is for filtering thick first to be processed
Cyclosiloxane；
3) filtered by filter cake in the thick methyl cyclosiloxane that organic silicon scrap cracking obtains being squeezed into pressure filter successively, mistake
Filter effect be thick methyl cyclosiloxane is neutralized, remove impurity, decolouring；
4) obtain fine work methyl cyclosiloxane after having filtered, be directly used in and prepare organosilicon downstream product, or for step
1) use as adjuvant in.
The process for purification of methyl cyclosiloxane the most according to claim 1, it is characterised in that: in pressure filter, filter cake occurs
When filtering slow, being opened by pressure filter, filter cake shovel is fallen, the filter cake after shoveling can mix in organic silicon scrap and crack, weight
Newly making filter cake, under normal circumstances, Primary batching system may filter that the thick methyl cyclosiloxane of 3-5 ton.
The process for purification of methyl cyclosiloxane the most according to claim 1, it is characterised in that: described pressure filter is one
10m2Plate and frame type filter-press.
The process for purification of methyl cyclosiloxane the most according to claim 1, it is characterised in that: described gear pump is one
The gear pump of 1.5 kilowatts.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310347812.9A CN103450249B (en) | 2013-08-12 | 2013-08-12 | The process for purification of methyl cyclosiloxane |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310347812.9A CN103450249B (en) | 2013-08-12 | 2013-08-12 | The process for purification of methyl cyclosiloxane |
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| CN103450249A CN103450249A (en) | 2013-12-18 |
| CN103450249B true CN103450249B (en) | 2016-09-14 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109553636B (en) * | 2017-09-27 | 2021-03-09 | 湖北兴瑞硅材料有限公司 | Impurity removal method for organic siloxane mixed ring body |
| CN115340567B (en) * | 2022-09-23 | 2024-03-29 | 鲁西化工集团股份有限公司硅化工分公司 | Method for improving quality of dimethylsiloxane mixed ring body product |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161969A (en) * | 1996-01-30 | 1997-10-15 | 拜尔公司 | Multifunctional cyclic organic siloxane, preparation method and usage thereof |
| CN1201796A (en) * | 1997-06-06 | 1998-12-16 | 吴世维 | Method for producing organic silicon rings from waste silicon rubber by pyrolysis |
| CN1699378A (en) * | 2005-06-09 | 2005-11-23 | 吴世维 | Process for preparing cyclic siloxane by using silicone rubber leftover materials |
| US20080009645A1 (en) * | 2005-12-07 | 2008-01-10 | Mindi Xu | Preparation Of Adsorbents For Purifying Organosilicon Compounds |
| CN101781401A (en) * | 2009-01-20 | 2010-07-21 | 扬州宏远化工新材料有限公司 | Novel method for producing hydroxy silicone oil |
-
2013
- 2013-08-12 CN CN201310347812.9A patent/CN103450249B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161969A (en) * | 1996-01-30 | 1997-10-15 | 拜尔公司 | Multifunctional cyclic organic siloxane, preparation method and usage thereof |
| CN1201796A (en) * | 1997-06-06 | 1998-12-16 | 吴世维 | Method for producing organic silicon rings from waste silicon rubber by pyrolysis |
| CN1699378A (en) * | 2005-06-09 | 2005-11-23 | 吴世维 | Process for preparing cyclic siloxane by using silicone rubber leftover materials |
| US20080009645A1 (en) * | 2005-12-07 | 2008-01-10 | Mindi Xu | Preparation Of Adsorbents For Purifying Organosilicon Compounds |
| CN101781401A (en) * | 2009-01-20 | 2010-07-21 | 扬州宏远化工新材料有限公司 | Novel method for producing hydroxy silicone oil |
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| CN103450249A (en) | 2013-12-18 |
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| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Refinement method of methylcyclosiloxane Effective date of registration: 20170929 Granted publication date: 20160914 Pledgee: China Postal Savings Bank Limited by Share Ltd Dongzhi County branch Pledgor: Dongzhi Oasis Environmental Protection Chemical Co., Ltd. Registration number: 2017340000257 |
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