CN108905304A - A kind of preparation method of organic silicon defoamer - Google Patents
A kind of preparation method of organic silicon defoamer Download PDFInfo
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- CN108905304A CN108905304A CN201811088538.7A CN201811088538A CN108905304A CN 108905304 A CN108905304 A CN 108905304A CN 201811088538 A CN201811088538 A CN 201811088538A CN 108905304 A CN108905304 A CN 108905304A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/02—Foam dispersion or prevention
- B01D19/04—Foam dispersion or prevention by addition of chemical substances
- B01D19/0404—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
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Abstract
The invention discloses a kind of preparation methods of organic silicon defoamer, this method is using silicon rubber production process intermediate pump condensation waste liquid as initial feed, by adsorb, synthesize and etc. obtain mixture, the mixing and emulsifyings such as the mixture and fumed silica, emulsifier, water are obtained into organic silicon defoamer.The present invention efficiently uses vacuum pump condensation collection liquid, and organic silicon waste liquid is converted into the organic silicon defoamer of high added value.Dimethicone is replaced with waste liquid synthetic product simultaneously, reduces the cost of organic silicon defoamer preparation.
Description
Technical field
The present invention relates to a kind of preparation methods of chemical assistant, specifically relate to a kind of preparation side of organic silicon defoamer
Method.
Background technique
Organosilicon enterprise can generate some siloxanes low molecule waste liquids when producing the downstream product such as silicon rubber at present, lead
Wanting source is that raw material dehydration and product take off roughing pump condensate liquid in silicon rubber production process, and main component is dimethyl silica
Alkane mixed methylcyclosiloxane, simultaneously containing impurity such as iron rust, lubricating oil.Iron rust, lubricating oil in the waste liquid can not be by simply handling
It removes, gained waste liquid cannot be used directly for production high-quality, the downstream product of high value.The waste liquid is usually outer to be sold for synthesizing one
A little coloured, flavored organosilicon low-end products, the level of resources utilization are low.
Organic silicon waste liquid usually passes through the methods of filtering, washing, rectifying and removes impurity, but filtering can only be in removing system not
Compatible impurity, washing can generate a large amount of industrial wastewaters, increase environmental protection pressure, rectifying cleans, and energy consumption is high, and cost is larger.
During many industrial productions, such as printing and dyeing, fermentation, papermaking, coating, medicine, oilfield exploitation, water process, by
A large amount of foams can be generated in operations such as stirring, vibration, boiling or addition auxiliary agents easy to foaming, if not appropriately processed, foam can be given
Production brings many troubles, such as influences being normally carried out, reduce equipment payload amount, causing product quality and production energy for production
Power decline etc..In order to eliminate and inhibit foam, the method for most effective and most economical simplicity is exactly that defoaming agent is added.Organosilicon defoaming
Agent is because its defoaming capacity is strong, thermal stability is good, plysiochemical strong inert, nontoxic, not generate the features such as secondary pollution wide
General application.Patent CN103830938A describes a kind of preparation method of organic silicon defoamer, by dimethicone and it is non-from
The components such as subtype surfactant under given conditions, are process through emulsification.Patent CN103877755A, which discloses one kind, to be had
Machine silicon defoaming agent and preparation method thereof, by dimethicone, hydroxy silicon oil, silica, aliphatic amine polyoxyethylene ether, hydrocarbonylation
Oil, emulsifier, thickener, water etc. by heating, stirring, heat preservation and etc. be prepared.Patent CN104225965A is disclosed
A kind of organic silicon defoamer and preparation method thereof is white by dimethicone, high boiling point silicon oil, thickener, water, emulsifier, gas phase
Carbon black etc. is mixed, emulsifies preparation.But the preparation of the organic silicon defoamer of the above patent report is all using silicone oil as primary raw material,
By the methods of stirring, emulsifying preparation, although patent CN104225965A utilizes high boiling point silicon oil, only by with
Methyl-silicone oil is used in compounding, and dosage is smaller, cannot be made full use of to organic silicon waste liquid, exhaust gas, higher cost.
Summary of the invention
Utilization rate in order to solve the problems, such as organic silicon waste liquid is low and organic silicon defoamer higher cost, by vacuum pump lime set
Iron rust, peculiar smell are removed by activated carbon adsorption, waste liquid and hexamethyldisiloxane mixing after absorption, in cation exchange resin
Catalysis under, carry out synthetic reaction, obtain the mixture of polysiloxanes and lubricating oil, using the mixture replace methyl-silicone oil system
Standby defoaming agent.
A kind of preparation method of organic silicon defoamer provided by the invention comprises the steps of：
(1) waste liquid that the condensation of silicon rubber production process intermediate pump is collected is decolourized using activated carbon adsorption, obtains product
A mixes product a with hexamethyldisiloxane, and reaction obtains product b under ring-opening polymerization catalyst effect, and product b is in 150-
Deviate from low molecule at 180 DEG C, preferably 160 DEG C, obtains product c；
(2) product c is added into reaction vessel, is warming up to 130-160 DEG C, gas-phase silica is added while stirring, wait stir
Continue stirring 3-6h after mixing uniformly and obtains silicon cream；
(3) silicon cream is added in container, is warming up to 50-70 DEG C, emulsifier and water are added while stirring, after mixing
With emulsifier 20-30min, organic silicon defoamer is obtained.
The dimethyl siloxane mixed methylcyclosiloxane that the ingredient for the waste liquid that the vacuum pump condensation is collected is 95-98%, 1-2%
Mechanical admixture, 1-3% lubricating oil.
The activated carbon adsorption condition is 15 DEG C -35 DEG C of temperature, adsorption time 10-30min.
The quality of the hexamethyldisiloxane is the 0.8-1.2% of product a mass, and ring-opening polymerization catalyst dosage is
The 4-8% of product a mass, reaction temperature are 60-90 DEG C, reaction time 2.5-4.5h.
The ring-opening polymerization catalyst is cation exchange resin, in tetramethylammonium hydroxide, potassium hydroxide, the concentrated sulfuric acid
Any one.
Gas-phase silica accounts for the 4-6% of product c mass in the step (2)；In step (3), silicon cream, emulsifier, water
Mass ratio be 1：0.05-0.08：8-10.
The emulsifier is the mixture of Span-80 and Tween-80, mass ratio 1:1-1.4.
The mulser mixing speed is 2500-3500r/min.The present invention compared with the existing technology the advantage is that：
1. the present invention efficiently uses vacuum pump condensation collection liquid, organic silicon waste liquid is converted into high added value
Organic silicon defoamer.
2. replacing dimethicone with waste liquid synthetic product, the cost of organic silicon defoamer synthesis is reduced.
3. containing partial lubrication oil component in waste liquid, certain defoaming can be played the role of, made full use of in waste liquid
Each ingredient.
Specific embodiment
Embodiment 1：
The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is adsorbed under conditions of 15 DEG C using active carbon
30min, waste liquid, hexamethyldisiloxane and cation exchange resin after absorption press 100:0.8:6 mass ratio mixing, 80 DEG C
Under conditions of reaction 4h obtain mixture, to 160 DEG C of mixture, 2h deviates from low molecule, obtains synthetic product.Into reaction vessel
The above-mentioned synthetic product of 100g is added, is warming up to 150 DEG C, is slowly added to 4g gas-phase silica while stirring, after being all added, stirs
3h is mixed to product in uniform paste, obtains silicon cream.It is in mass ratio 1:1 ratio mixing Span-80 and Tween-80 is as cream
Agent.100g silicon cream is added in container, and is warming up to 60 DEG C, 800g water is added while stirring, 5g emulsifier is then added,
3500r/min emulsifies 20min and obtains organic silicon defoamer after mixing.
Embodiment 2：
The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is adsorbed under conditions of 25 DEG C using active carbon
25min, waste liquid, hexamethyldisiloxane and cation exchange resin after absorption press 100:0.8:4 mass ratio mixing, 90 DEG C
Under conditions of reaction 4.5h obtain mixture, to 160 DEG C of mixture, 2h deviates from low molecule, obtains synthetic product.To reaction vessel
The above-mentioned synthetic product of middle addition 100g, is warming up to 150 DEG C, is slowly added to 5g gas-phase silica while stirring, after being all added,
It is in uniform paste that 4.5h, which is stirred, to product, obtains silicon cream.It is in mass ratio 1:1.1 ratio mixes Span-80 and Tween-80
As emulsifier.100g silicon cream is added in container, and is warming up to 60 DEG C, 850g water is added while stirring, 6g is then added
Emulsifier, 3000r/min emulsifies 25min and obtains organic silicon defoamer after mixing.
Embodiment 3：
The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is adsorbed under conditions of 35 DEG C using active carbon
15min, waste liquid, hexamethyldisiloxane and potassium hydroxide after absorption press 100:1:6 mass ratio mixes, under conditions of 80 DEG C
Reaction 3h obtains mixture, and to 160 DEG C of mixture, 2h deviates from low molecule, obtains synthetic product.100g is added into reaction vessel
Above-mentioned synthetic product, is warming up to 150 DEG C, is slowly added to 6g gas-phase silica while stirring, after being all added, stirring 6h to production
Product are in uniform paste, obtain silicon cream.It is in mass ratio 1:1.2 ratio mixing Span-80 and Tween-80 is as emulsifier.It will
100g silicon cream is added in container, and is warming up to 60 DEG C, and 950g water is added while stirring, and 7g emulsifier is then added, and mixing is equal
2500r/min emulsification 30min obtains organic silicon defoamer after even.
Embodiment 4：
The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is adsorbed under conditions of 25 DEG C using active carbon
25min, waste liquid, hexamethyldisiloxane and tetramethylammonium hydroxide after absorption press 100:1.2:8 mass ratio mixing, 60 DEG C
Under conditions of reaction 3.5h obtain mixture, to 160 DEG C of mixture, 2h deviates from low molecule, obtains synthetic product.To reaction vessel
The above-mentioned synthetic product of middle addition 100kg, is warming up to 150 DEG C, is slowly added to 5kg gas-phase silica while stirring, to whole additions
Afterwards, stirring 4.5h is in uniform paste to product, obtains silicon cream.It is in mass ratio 1:1.3 ratio mixes Span-80 and Tween-
80 are used as emulsifier.100kg silicon cream is added in container, and is warming up to 60 DEG C, while stirring be added 1000kg water, then plus
Enter 8kg emulsifier, 3000r/min emulsifies 30min and obtains organic silicon defoamer after mixing.
Embodiment 5：
The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is adsorbed under conditions of 25 DEG C using active carbon
25min, waste liquid, hexamethyldisiloxane and the concentrated sulfuric acid after absorption press 100:1.0:8 mass ratio mixes, under conditions of 80 DEG C
Reaction 2.5h obtains mixture, and to 160 DEG C of mixture, 2h deviates from low molecule, obtains synthetic product.It is added into reaction vessel
The above-mentioned synthetic product of 100kg, is warming up to 150 DEG C, is slowly added to 5kg gas-phase silica while stirring, after being all added, stirring
4.5h is in uniform paste to product, obtains silicon cream.It is in mass ratio 1:1.4 ratio mixes Span-80 and Tween-80 conduct
Emulsifier.100kg silicon cream is added in container, and is warming up to 60 DEG C, 950kg water is added while stirring, 7kg cream is then added
Agent, 3000r/min emulsifies 30min and obtains organic silicon defoamer after mixing.
Embodiment 6：
The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is adsorbed under conditions of 25 DEG C using active carbon
25min, waste liquid, hexamethyldisiloxane and cation exchange resin after absorption press 100:0.9:6 mass ratio mixing, 80 DEG C
Under conditions of reaction 4h obtain mixture, to 160 DEG C of mixture, 2h deviates from low molecule, obtains synthetic product.Into reaction vessel
The above-mentioned synthetic product of 100kg is added, is warming up to 150 DEG C, is slowly added to 5kg gas-phase silica while stirring, after being all added,
It is in uniform paste that 4.5h, which is stirred, to product, obtains silicon cream.It is in mass ratio 1:1.2 ratio mixes Span-80 and Tween-80
As emulsifier.100kg silicon cream is added in container, and is warming up to 60 DEG C, 950kg water is added while stirring, is then added
7kg emulsifier, 3000r/min emulsifies 30min and obtains organic silicon defoamer after mixing.
Comparative example 1
100 parts of 500mpa.s methyl-silicone oils are added into reaction vessel, is warming up to 150 DEG C, is slowly added to 5 parts while stirring
Gas-phase silica, after being all added, stirring 4.5h to product is in uniform paste, obtains silicon cream.It is in mass ratio 1:1.2 ratio
Span-80 and Tween-80 is as emulsifier for example mixing.100 parts of silicon cream are added in container, and are warming up to 60 DEG C, side stirring
950 parts of water are added in side, and 7 parts of emulsifiers are then added, and 3000r/min emulsifies 30min and obtains organic silicon defoamer after mixing.
Comparative example 2
100 parts of 1000mpa.s methyl-silicone oils are added into reaction vessel, is warming up to 150 DEG C, is slowly added to 5 while stirring
Part gas-phase silica, after being all added, stirring 4.5h to product is in uniform paste, obtains silicon cream.It is in mass ratio 1:1.4
Ratio mixes Span-80 and Tween-80 as emulsifier.100 parts of silicon cream are added in container, and are warming up to 60 DEG C, while stirring
It mixes side and 950 parts of water is added, 7 parts of emulsifiers are then added, 3000r/min emulsifies 30min and obtains organosilicon defoaming after mixing
Agent.
Antifoam performance detection：
The antifoam performance of defoaming agent in above-described embodiment and comparative example is tested according to GB/T26527-2011, as a result such as table 1：
1. defoaming agent antifoam performance contrast table of table
Claims (8)
1. a kind of preparation method of organic silicon defoamer, which is characterized in that comprise the steps of：
（1）The waste liquid that the condensation of silicon rubber production process intermediate pump is collected is decolourized using activated carbon adsorption, obtains product a, it will
Product a is mixed with hexamethyldisiloxane, and reaction obtains product b under ring-opening polymerization catalyst effect, and product b is in 150-170
Deviate from low molecule at DEG C, obtains product c；
（2）Product c is added into reaction vessel, is warming up to 130-160 DEG C, gas-phase silica is added while stirring, it is to be mixed equal
Continue stirring 3-6h after even and obtains silicon cream；
（3）By step（3）The silicon cream is added in container, is warming up to 50-70 DEG C, and emulsifier and water are added while stirring,
Emulsifier 20-30min is used after mixing, obtains organic silicon defoamer.
2. organic silicon defoamer preparation method as described in claim 1, which is characterized in that the waste liquid that vacuum pump condensation is collected
Ingredient is the dimethyl siloxane mixed methylcyclosiloxane of 95-98%, the mechanical admixture of 1-2%, 1-3% lubricating oil.
3. organic silicon defoamer preparation method as described in claim 1, which is characterized in that activated carbon adsorption condition is temperature 15
DEG C -35 DEG C, adsorption time 10-30min.
4. organic silicon defoamer preparation method as described in claim 1, which is characterized in that the quality of hexamethyldisiloxane is
The 0.8-1.2% of product a mass, ring-opening polymerization catalyst dosage are the 4-8% of product a mass, and reaction temperature is 60-90 DEG C, instead
2.5-4.5h obtains product b between seasonable, and product b deviates from low molecule at 160 DEG C and obtains product c.
5. organic silicon defoamer preparation method as described in claim 1, which is characterized in that the ring-opening polymerization catalyst is
Cation exchange resin, tetramethylammonium hydroxide, potassium hydroxide, any one in the concentrated sulfuric acid.
6. organic silicon defoamer preparation method as described in claim 1, which is characterized in that step（2）Middle gas-phase silica accounts for
The 4-6% of product c mass；Step（3）In, silicon cream, emulsifier, water mass ratio be 1：0.05-0.08：8-10.
7. organic silicon defoamer preparation method as described in claim 1, which is characterized in that the emulsifier be Span-80 and
The mixture of Tween-80, mass ratio 1:1-1.4.
8. organic silicon defoamer preparation method as described in claim 1, which is characterized in that mulser mixing speed is 2500-
3500r/min。
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1641097A (en) * | 2004-12-10 | 2005-07-20 | 曹治平 | Moderate temperature prnited and dyed organosilicon anti-bubbling and its preparing method |
| CN102343165A (en) * | 2011-10-20 | 2012-02-08 | 山东大易化工有限公司 | Efficient silicone defoaming agent |
| CN104225965A (en) * | 2014-09-24 | 2014-12-24 | 湖北兴瑞化工有限公司 | Organosilicone defoamer and preparation method thereof |
| CN105504290A (en) * | 2015-12-24 | 2016-04-20 | 开封中节能再生能源有限公司 | Antifoaming agent for household garbage leachate treatment system and desulfurization slurry foam |
-
2018
- 2018-09-18 CN CN201811088538.7A patent/CN108905304B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1641097A (en) * | 2004-12-10 | 2005-07-20 | 曹治平 | Moderate temperature prnited and dyed organosilicon anti-bubbling and its preparing method |
| CN102343165A (en) * | 2011-10-20 | 2012-02-08 | 山东大易化工有限公司 | Efficient silicone defoaming agent |
| CN104225965A (en) * | 2014-09-24 | 2014-12-24 | 湖北兴瑞化工有限公司 | Organosilicone defoamer and preparation method thereof |
| CN105504290A (en) * | 2015-12-24 | 2016-04-20 | 开封中节能再生能源有限公司 | Antifoaming agent for household garbage leachate treatment system and desulfurization slurry foam |
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Effective date of registration: 20221207 Address after: 431700 Road 12, yuekou Industrial Park, Tianmen City, Hubei Province Patentee after: HUBEI HUANYU CHEMICAL Co.,Ltd. Address before: 443007 No. 66-2 Ting Ting Road, Ting Ting District, Yichang, Hubei Patentee before: HUBEI XINGRUI SILICON MATERIAL Co.,Ltd. |
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