CN105688452B - A kind of emulsion-type organic silicon defoamer and preparation method thereof - Google Patents
A kind of emulsion-type organic silicon defoamer and preparation method thereof Download PDFInfo
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- CN105688452B CN105688452B CN201610241212.8A CN201610241212A CN105688452B CN 105688452 B CN105688452 B CN 105688452B CN 201610241212 A CN201610241212 A CN 201610241212A CN 105688452 B CN105688452 B CN 105688452B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
Abstract
The invention discloses a kind of emulsion-type organic silicon defoamer and preparation method thereof, it is at 90 100 DEG C, after being pre-processed with water repellent agent and ammonium dihydrogen phosphate to hydrophobic type gas-phase silica, obtained gas-phase silica and dimethicone are blended at 170 200 DEG C and obtain silicon cream, again in the presence of compound emulsifying agent, silicon cream, fatty alcohol and sodium phosphate are compounded to obtain the emulsion-type organic silicon defoamer.Instant invention overcomes the shortcomings that existing emulsion-type organic silicon defoamer easy in inactivation and suds suppressing properties difference, gained organic silicon defoamer has excellent alkaline-resisting and good continuous application performance, and its antifoaming speed is fast, suds suppressing properties are good, good emulsion stability, the defoaming activity time is grown, and preparation process clean environment firendly, discharge without " three wastes ", it is adapted to industrialized production.
Description
Technical field
The invention belongs to chemical technology field, and in particular to a kind of emulsion-type organic silicon defoamer and preparation method thereof.
Background technology
In the Industrial Engineering such as dyeing and weaving, food fermentation, pharmaceuticals industry, petrochemical industry, papermaking, wastewater treatment, it has been also easy to produce
Evil foam, not only influences production efficiency, causes the waste of raw material, also product quality is reduced.Therefore, need in the industrial production
Add defoamer and eliminate unwanted bubbles.
In the development course of defoamer, organosilicon emulsion-type defoamer is because its surface tension is small, heat endurance and chemistry
Stability is good, have the advantages that physiology and reactionlessness, higher defoaming activity are widely used in detergent, papermaking, sugaring, electricity
The industries such as plating, chemical fertilizer, wastewater treatment.But organosilicon emulsion-type defoamer equally exists deficiency, as suds suppressing properties are poor,
Easily failed in the continuous foamed system such as papermaking, wastewater treatment, sugaring；Defoaming is lost in application process because of disproportionation to live
Property, while the silicone oil isolated is also easy to be attached to fabric face and influence its outward appearance.
The present invention is transformed the formula of organosilicon composite anti-foaming agent, by increasing hydrophobic gas-phase silica and dimethyl
The adhesion of silicone oil strengthens its durability, increases its defoaming activity time in papermaking, dyeing process；And add other defoamings
Active component and organosilicon progress are compound, and to increase its spreading coefficient, reduction enters potential barrier, further speeds up antifoaming speed, increases
The suds suppressing properties of big organosilicon composite anti-foaming agent, while the usage amount of organosilicon is reduced, reduce silicone oil and be attached to fabric, paper table
Face rings the possibility of outward appearance；The component of foam aging can be accelerated by adding, and be cooperateed with other active components of composite anti-foaming agent
Defoaming, accelerates disintegrating for foam.
The content of the invention
It is an object of the invention to provide a kind of emulsion-type organic silicon defoamer and preparation method thereof, the defoaming of gained organosilicon
Faster, suds ability is stronger, and action time is more longlasting for agent antifoaming speed, and cost is more cheap, is that a New Emulsion type is organic
Silicon defoaming agent.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of emulsion-type organic silicon defoamer, its preparation method comprise the following steps：
1）The processing of hydrophobic type gas-phase silica：Hydrophobic type gas-phase silica, ammonium dihydrogen phosphate and water repellent agent are existed
The h of insulation reaction 1 at 90-100 DEG C, the gas-phase silica after must handling；
2）The preparation of silicon cream：Gas-phase silica after processing is incubated with dimethicone at 170-200 DEG C and mixed
2.5-3 h, obtain silicon cream；
3）Emulsification compounding：By step 2）Obtained silicon cream is with fatty alcohol, sodium phosphate, compound emulsifying agent under the conditions of 75 DEG C
It is well mixed, phase inversion is then slowly added water at 70 DEG C, remaining water is added after stirring 20 min, continues to stir 20 min
Stop heating afterwards, be cooled to after room temperature to discharge and produce.
Step 1）In raw materials used be calculated as by weight：100 parts of hydrophobic type gas-phase silica, ammonium dihydrogen phosphate 3-5 parts, dredge
Water treatment agent 3-5 parts.Wherein, the specific surface area of the hydrophobic type gas-phase silica is 225-275m2/g；The water repellent agent
For one or both of HMDS, 1- octanols.
Step 2）In raw materials used be calculated as by weight：2 parts of gas-phase silica, 48 parts of dimethicone.Wherein, described two
The viscosity of methyl-silicone oil is 500-1000 mPas.
Step 3）In raw materials used be calculated as by weight：Silicon cream 70-80 parts, fatty alcohol 20-30 parts, sodium phosphate 5-10 parts,
Compound emulsifying agent 26-32 parts, water 500-550 parts.Wherein, the compound emulsifying agent is by octadecyl alcolol, monoglyceride, Arlacel-60, told
Temperature -60, isomeric alcohol polyethenoxy ether are by weight 8:2:8:6:2 mix；The fatty alcohol is that main chain contains 6-8 carbon atom
One or both of fatty alcohol, including 1- octanols, 1- hexanols, isooctanol.
Compared with prior art, the emulsion-type organic silicon defoamer that prepared by the present invention has following advantage：
1）Through water repellent agent with it is phosphate-modified after hydrophobic gas-phase silica and dimethicone adhesion it is bigger,
The phase rich in silicone oil is disproportionated into continuous defoaming circulation and the speed rich in white carbon phase is slower, acts on its defoaming
It is more longlasting；
2）The addition of fatty alcohol increases the spreading coefficient of organic silicon defoamer, reduces the entrance potential barrier of defoamer, and
Vacuolar membrane surface forms loose unstable film surface, accelerates the rupture of vacuolar membrane；
3）Phosphatic addition at high price, the charge stable on vacuolar membrane surface can be destroyed, accelerate the aging of vacuolar membrane to merge, and and its
His component plays a part of collaboration defoaming；
4）The synergy of fatty alcohol, high price salt and silicon cream, gained defoamer antifoaming speed can be made faster；
5）Considered in terms of production cost, it is all common chemical products that it is raw materials used, which to prepare defoamer of the present invention, and is disappeared
Composition of the infusion more than 80% is water, greatly reduces production cost, decreases the pollution to environment in preparation process.
Brief description of the drawings
Fig. 1 is the volume time history plot of foam solution in antifoam performance test.
Fig. 2 is the cycle performance test chart of the defoamer of embodiment 3.
Fig. 3 is the cycle performance test chart of the defoamer of comparative example 1.
Fig. 4 is the cycle performance test chart of the defoamer of comparative example 2.
Embodiment
A kind of emulsion-type organic silicon defoamer, its preparation method comprise the following steps：
1）The processing of hydrophobic type gas-phase silica：By 100 parts by weight hydrophobic type gas-phase silicas, 3-5 parts by weight of phosphoric acid two
Hydrogen ammonium and 3-5 parts by weight water repellent agent h of insulation reaction 1 at 90-100 DEG C, the gas-phase silica after must handling；
2）The preparation of silicon cream：By the gas-phase silica after the processing of 2 parts by weight and 48 parts by weight dimethicones in 170-200
Insulation mixing 2.5-3 h, obtain silicon cream at DEG C；
3）Emulsification compounding：In four-hole boiling flask, by 70-80 parts by weight steps 2）Obtained silicon cream, 20-30 parts by weight fat
Alcohol, 5-10 parts by weight of phosphoric acid sodium, 26-32 parts by weight compound emulsifying agent are well mixed under the conditions of 75 DEG C, are then delayed at 70 DEG C
Slowly plus 200-300 parts by weight water is to phase inversion, adds 250-300 parts by weight water after stirring 20 min, continues to stir 20 min
Stop heating afterwards, be cooled to after room temperature to discharge and produce.
Step 1）Described in the specific surface area of hydrophobic type gas-phase silica be 225-275m2/g；The water repellent agent is
One or both of HMDS, 1- octanols.
Step 2）Described in the viscosity of dimethicone be 500-1000 mPas.
Step 3）Described in compound emulsifying agent be by octadecyl alcolol, monoglyceride, Arlacel-60, Tween-60, isomery alcohol polyoxy second
Alkene ether is by weight 8:2:8:6:2 mix；The fatty alcohol be fatty alcohol of the main chain containing 6-8 carbon atom in one kind or
Two kinds, including 1- octanols, 1- hexanols, isooctanol.
In order that content of the present invention easily facilitates understanding, with reference to embodiment to of the present invention
Technical scheme is described further, but the present invention is not limited only to this.
Embodiment 1：
1）The processing of hydrophobic type gas-phase silica：By 100 parts by weight hydrophobic type gas-phase silicas（Specific surface area is 225m2/
g）, 3 parts by weight of phosphoric acid ammonium dihydrogens and 3 parts by weight 1- the octanols h of insulation reaction 1 at 95 DEG C, the gas-phase silica after must handling；
2）The preparation of silicon cream：By the gas-phase silica and 48 parts by weight dimethicones after the processing of 2 parts by weight（Viscosity 1000
mPa·s）2.5 h of insulation mixing, obtain silicon cream at 180 DEG C；
3）Emulsification compounding：In four-hole boiling flask, by 70 parts by weight steps 2）Obtained silicon cream, 30 parts by weight 1- octanols, 5 weights
Measure part sodium phosphate, 9.8 parts by weight octadecyl alcolols, 2.5 parts by weight monoglycerides, 9.8 parts by weight Arlacel-60s, 7.4 parts by weight Tween-60s,
2.5 parts by weight isomeric alcohol polyethenoxy ethers are well mixed under the conditions of 75 DEG C, and 200 parts by weight are then slowly added at 70 DEG C
Water adds 300 parts by weight water after stirring 20 min, continues to stop heating after stirring 20 min, after being cooled to room temperature to phase inversion
Discharge and produce.
Embodiment 2：
1）The processing of hydrophobic type gas-phase silica：By 100 parts by weight hydrophobic type gas-phase silicas（Specific surface area is 275m2/
g）, 4 parts by weight of phosphoric acid ammonium dihydrogens and 4 parts by weight the HMDSs h of insulation reaction 1 at 100 DEG C, the gas after must handling
Phase white carbon；
2）The preparation of silicon cream：By the gas-phase silica and 48 parts by weight dimethicones after the processing of 2 parts by weight（Viscosity 800
mPa·s）2.5 h of insulation mixing, obtain silicon cream at 200 DEG C；
3）Emulsification compounding：In four-hole boiling flask, by 75 parts by weight steps 2）Obtained silicon cream, 25 parts by weight isooctanol, 10
Parts by weight of phosphoric acid sodium, 8 parts by weight octadecyl alcolols, 2 parts by weight monoglycerides, 8 parts by weight Arlacel-60s, 6 parts by weight Tween-60s, 2 weight
Part isomeric alcohol polyethenoxy ether is well mixed under the conditions of 75 DEG C, then slowly adds 300 parts by weight water extremely to turn at 70 DEG C
Phase, 250 parts by weight water are added after stirring 20 min, continue to stop heating after stirring 20 min, discharged i.e. after being cooled to room temperature
.
Embodiment 3：
1）The processing of hydrophobic type gas-phase silica：By 100 parts by weight hydrophobic type gas-phase silicas（Specific surface area is 250m2/
g）, 5 parts by weight of phosphoric acid ammonium dihydrogens and 5 parts by weight the HMDSs h of insulation reaction 1 at 90 DEG C, the gas after must handling
Phase white carbon；
2）The preparation of silicon cream：By the gas-phase silica and 48 parts by weight dimethicones after the processing of 2 parts by weight（Viscosity 500
mPa·s）3 h of insulation mixing, obtain silicon cream at 200 DEG C；
3）Emulsification compounding：In four-hole boiling flask, by 80 parts by weight steps 2）Obtained silicon cream, 20 parts by weight 1- hexanols, 8 weights
Measure part sodium phosphate, 8 parts by weight octadecyl alcolols, 2 parts by weight monoglycerides, 8 parts by weight Arlacel-60s, 6 parts by weight Tween-60s, 2 parts by weight
Isomeric alcohol polyethenoxy ether is well mixed under the conditions of 75 DEG C, then at 70 DEG C slowly plus 260 parts by weight water are to phase inversion,
270 parts by weight water are added after stirring 20 min, continue to stop heating after stirring 20 min, is cooled to after room temperature to discharge and produces.
Comparative example 1：
1）The processing of hydrophobic type gas-phase silica：By 100 parts by weight hydrophobic type gas-phase silicas（Specific surface area is 250m2/
g）, 2 parts by weight of phosphoric acid ammonium dihydrogens and 4 parts by weight the HMDSs h of insulation reaction 1 at 90 DEG C, the gas after must handling
Phase white carbon；
2）The preparation of silicon cream：By the gas-phase silica and 48 parts by weight dimethicones after the processing of 2 parts by weight（Viscosity 500
mPa·s）3 h of insulation mixing, obtain silicon cream at 200 DEG C；
3）Emulsification compounding：In four-hole boiling flask, by 80 parts by weight steps 2）Obtained silicon cream, 20 parts by weight 1- hexanols, 8 weights
Measure part octadecyl alcolol, 2 parts by weight monoglycerides, 8 parts by weight Arlacel-60s, 6 parts by weight Tween-60s, 2 parts by weight isomery alcohol polyoxyethylene
Ether is well mixed under the conditions of 75 DEG C, then at 70 DEG C slowly plus 260 parts by weight water are to phase inversion, is stirred after 20 min again
270 parts by weight water are added, continue to stop heating after stirring 20 min, is cooled to after room temperature to discharge and produces.
Comparative example 2：
1）The preparation of silicon cream：By 2 parts by weight hydrophobic type gas-phase silicas（Specific surface area is 250m2/g）With 48 parts by weight two
Methyl-silicone oil（The mPas of viscosity 500）3 h of insulation mixing, obtain silicon cream at 200 DEG C；
2）Emulsification compounding：In four-hole boiling flask, by 80 parts by weight steps 1）Obtained silicon cream, 20 parts by weight 1- hexanols, 8 weights
Measure part octadecyl alcolol, 2 parts by weight monoglycerides, 8 parts by weight Arlacel-60s, 6 parts by weight Tween-60s, 2 parts by weight isomery alcohol polyoxyethylene
Ether is well mixed under the conditions of 75 DEG C, then at 70 DEG C slowly plus 260 parts by weight water are to phase inversion, is stirred after 20 min again
270 parts by weight water are added, continue to stop heating after stirring 20 min, is cooled to after room temperature to discharge and produces.
Defoamer cycle performance is tested：
Key instrument device：Bubbler, 500 mL tool plug graduated cylinders；
Test condition：25 DEG C of temperature
Tested media：Standard foam liquid
Specific method of testing：Weigh 0.44g neopelexes and be dissolved in 100 mL water stirring to transparence liquid
As standard foam liquid；100 mL standard foam liquids are poured into 500 mL graduated cylinders, after adding 10 μ L defoamers, use bubbler
Bubble and the time of the removal of foam, the defoaming cycle performance test result as defoamer are recorded after 10 s.
Fig. 1 is embodiment 3 and comparative example 1, the volume of 2 gained defoamers foam solution in antifoam performance test anaplasia at any time
The curve map of change.From figure 1 it appears that with the extension of cream time, the foam of the foam liquid of the addition defoamer of embodiment 3
Volume will be far smaller than the foam volume of comparative example 1 and comparative example 2.
Fig. 2,3,4 are respectively the cycle performance test chart of embodiment 3, comparative example 1 and the gained defoamer of comparative example 2.From figure
In as can be seen that comparative example 2 defoamer by 30 times defoaming circulation after, foam time is greater than 60s；Comparative example 1 passes through 80
Foam time is also greater than 60 s after secondary circulation；And the defoamer of embodiment 3 by 120 times defoaming circulation after, foam time according to
So it is less than 60 s.Thus prove, silicon made of the gas-phase silica of the invention by after ammonium dihydrogen phosphate and water repellent agent processing
There is obvious growth the defoaming activity time for the organic silicon defoamer that cream and sodium ascorbyl phosphate are prepared, and antifoaming speed is fast,
Stable performance, it is adapted to industrialized production.
The foregoing is only presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, it should all belong to the covering scope of the present invention.
Claims (8)
- A kind of 1. preparation method of emulsion-type organic silicon defoamer, it is characterised in that：Comprise the following steps：1）The processing of hydrophobic type gas-phase silica：By hydrophobic type gas-phase silica, ammonium dihydrogen phosphate and water repellent agent in 90- The h of insulation reaction 1 at 100 DEG C, the gas-phase silica after must handling；The water repellent agent is 1- octanols；2）The preparation of silicon cream：Gas-phase silica after processing is incubated with dimethicone at 170-200 DEG C and mixes 2.5-3 H, obtain silicon cream；3）Emulsification compounding：By step 2）Obtained silicon cream mixes with fatty alcohol, sodium phosphate, compound emulsifying agent under the conditions of 75 DEG C Uniformly, phase inversion is then slowly added water at 70 DEG C, remaining water is added after stirring 20 min, continues to stop after stirring 20 min Only heat, be cooled to after room temperature to discharge and produce.
- 2. the preparation method of emulsion-type organic silicon defoamer according to claim 1, it is characterised in that：Step 1）In original used Material is calculated as by weight：100 parts of hydrophobic type gas-phase silica, ammonium dihydrogen phosphate 3-5 parts, water repellent agent 3-5 parts.
- 3. the preparation method of emulsion-type organic silicon defoamer according to claim 2, it is characterised in that：The hydrophobic type gas phase The specific surface area of white carbon is 225-275m2/g。
- 4. the preparation method of emulsion-type organic silicon defoamer according to claim 1, it is characterised in that：Step 2）In original used Material is calculated as by weight：2 parts of gas-phase silica, 48 parts of dimethicone.
- 5. the preparation method of emulsion-type organic silicon defoamer according to claim 4, it is characterised in that：The dimethyl-silicon The viscosity of oil is 500-1000 mPas.
- 6. the preparation method of emulsion-type organic silicon defoamer according to claim 1, it is characterised in that：Step 3）In original used Material is calculated as by weight：Silicon cream 70-80 parts, fatty alcohol 20-30 parts, sodium phosphate 5-10 parts, compound emulsifying agent 26-32 parts, water 500-550 parts.
- 7. the preparation method of emulsion-type organic silicon defoamer according to claim 6, it is characterised in that：The compound emulsifying agent It is by weight 8 by octadecyl alcolol, monoglyceride, Arlacel-60, Tween-60, isomeric alcohol polyethenoxy ether:2:8:6:2 mix.
- 8. the preparation method of emulsion-type organic silicon defoamer according to claim 6, it is characterised in that：Based on the fatty alcohol One or both of the fatty alcohol of chain containing 6-8 carbon atom, including 1- octanols, 1- hexanols, isooctanol.
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Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106267910A (en) * | 2016-08-10 | 2017-01-04 | 中国海洋石油总公司 | A kind of defoamer and its production and use |
| CN106422430A (en) * | 2016-11-01 | 2017-02-22 | 合肥新万成环保科技有限公司 | Environment-friendly organic silicon defoamer |
| CN106334348A (en) * | 2016-11-01 | 2017-01-18 | 合肥新万成环保科技有限公司 | Compound defoaming agent capable of improving toughness |
| CN106540477A (en) * | 2016-11-01 | 2017-03-29 | 合肥新万成环保科技有限公司 | A kind of defoamer with fire retardation |
| CN106362442A (en) * | 2016-11-01 | 2017-02-01 | 合肥新万成环保科技有限公司 | Waterproof polyether formulated de-foaming agent |
| CN106390533A (en) * | 2016-11-01 | 2017-02-15 | 合肥新万成环保科技有限公司 | Organosilicon defoamer with bactericidal action |
| CN106377927A (en) * | 2016-11-01 | 2017-02-08 | 合肥新万成环保科技有限公司 | Organic silicon antifoaming agent containing nano powder |
| CN106362444A (en) * | 2016-11-01 | 2017-02-01 | 合肥新万成环保科技有限公司 | Composite organic silicon defoamer containing coconut oil |
| CN106512486A (en) * | 2016-11-01 | 2017-03-22 | 合肥新万成环保科技有限公司 | Compound polyether defoaming agent capable of ultraviolet ray protection |
| CN106563293A (en) * | 2016-11-01 | 2017-04-19 | 合肥新万成环保科技有限公司 | A high-strength compound defoamer |
| CN106362443A (en) * | 2016-11-01 | 2017-02-01 | 合肥新万成环保科技有限公司 | Organic silicon defoaming agent with anti-cracking function |
| CN110064233A (en) * | 2019-04-29 | 2019-07-30 | 宜昌汇富硅材料有限公司 | Organic silicon defoamer and preparation method thereof |
| CN110548315A (en) * | 2019-08-14 | 2019-12-10 | 湖南登科材料科技有限公司 | Novel organic silicon defoaming agent and preparation method thereof |
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| GB0219073D0 (en) * | 2002-08-16 | 2002-09-25 | Dow Corning | Silicone foam control compositions |
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| CN1613537A (en) * | 2004-09-22 | 2005-05-11 | 曹治平 | High-temperature defoamer and its preparation |
| CN102961896A (en) * | 2011-11-17 | 2013-03-13 | 天津法莫西医药科技有限公司 | Powder defoaming agent with flyash hollow glass beads as filler |
| CN104069654A (en) * | 2014-07-01 | 2014-10-01 | 西安道尔达化工有限公司 | Preparation method of high-viscosity organic silicon defoamer |
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