CN106474775A - A kind of hyperbranched polyether modified organic silicon defoamer of nano-silica-containing and preparation method thereof - Google Patents
A kind of hyperbranched polyether modified organic silicon defoamer of nano-silica-containing and preparation method thereof Download PDFInfo
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- CN106474775A CN106474775A CN201610904645.7A CN201610904645A CN106474775A CN 106474775 A CN106474775 A CN 106474775A CN 201610904645 A CN201610904645 A CN 201610904645A CN 106474775 A CN106474775 A CN 106474775A
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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
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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
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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
- B01D19/0427—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing halogen-atoms
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Abstract
The present invention discloses a kind of hyperbranched polyether modified organic silicon defoamer of nano-silica-containing, is made up of the raw material of following weight portion：25 40 parts of polysiloxanes, 13 23 parts of hyperbranched polyether, 16 26 parts of allyl glycidyl ether, 38 58 parts of expoxy propane, 0.3 0.5 parts of bimetallic cyaniding complex, 50 70 parts of isopropanol, 0.2 0.5 parts of chloroplatinic acid catalyst, 26 parts of superfine alumina silicate, 12 parts of D-sorbite, 12 parts of polysorbate60,24 parts of sodium carboxymethylcellulose, appropriate deionized water, 4 11 parts of nano grade silica particles, 45 60 parts of dodecanol.The present invention contains the hyperbranched polyether of great amount of hydroxy group as raw material with end, prepare end-allyl group hyperbranched polyether, there is hydrosilylation using the double bond structure and polysiloxanes of modified polyether end group, synthesis of super branched Siloxane-Oxyalkylene Copolymers, the defoamer in order to prepare have excellent anti-shear performance.
Description
Technical field
The present invention relates to chemicals field, the hyperbranched polyether modification of more particularly to a kind of nano-silica-containing is organic
Silicon defoaming agent and preparation method thereof.
Technical background
Defoamer, is also called defrother or foamicide, can produce the bubble of many impact productions during industrial production
Foam, needs to add defoamer.It is widely used in removing latex, textile sizing, food fermentation, biological medicine, coating, oil
The unwanted bubbles produced during the industry production such as work, papermaking, industry cleaning link, sewage disposal.
Existing defoamer can be divided into organic silicon type and two big class of polyether-type according to composition, and organic silicon defoamer is due to emulsification
The addition of the auxiliary agents such as agent, easily occurs the defects such as breakdown of emulsion, floating oil at relatively high temperatures；Polyether-type defoamer be mostly by initiator and
The polymer that oxirane, expoxy propane ring-opening polymerisation are formed, its maximum advantage are that suds power is strong, but fatal defects are brokenly bubbles
Rate is low, and froth breaking is not slowly thorough.Higher with regard to the new applicability of exploitation in recent years, the research layer of the higher defoamer of defoaming effectiveness
Go out not poor.Polyether modified polysiloxan defoaming agent passes through to introduce polyether segment on silicone oil segment, common so as to have two kinds of defoamers concurrently
Advantage, froth breaking effect is strong, and heat resistance, shear resistant and acid-proof alkaline are good.But the polyether modified silicon oil of research disappears at present
Infusion is not satisfactory in terms of anti-shear performance, limits its application on some fields such as coating, petrochemical industry, papermaking.
Dissaving polymer is the highly branched macromolecular that a class has torispherical structure, containing a large amount of functional end-groups,
Have the characteristics that low melt and solution viscosity.After linear polymer is sheared, molecular backbone is interrupted, under causing molecular weight significantly
Drop, and after dissaving polymer is sheared, can interrupt a certain branched structure, not interfere with main chain performance, therefore hyperbranched polymerization
Thing can have more preferable anti-shear ability than linear polymer in theory.
Xu Junqi, Huang Tong, Lv Xin et al. are at which《The synthesis of water-soluble high shear hyperbranched poly acrylamide and sign》
In one text, raw radical polymerization is issued in cerium salt-hydroxyl initiator system with hyperbranched polyglycidyl ether, acrylamide, is obtained
Highly branched water-soluble ultrabranching polyacrylamide HPG-star-PAM, as a result shows highly branched polyacrylamide sample
Product have excellent anti-shear performance.
Therefore, the present invention is by preparing end-allyl group hyperbranched poly ethoxylated polyhydric alcohol to the terminal groups modification of hyperbranched polyether, profit
There is hydrosilylation with the double bond structure and polysiloxanes of modified hyperbranched polyether, prepare hyperbranched polyether modified poly-
Siloxanes, improves anti-shear performance, the froth breaking suds suppressing properties of defoamer.
Content of the invention
For the deficiencies in the prior art, the present invention provides a kind of hyperbranched polyether modified organic silicon of nano-silica-containing
Defoamer and preparation method thereof.
A kind of hyperbranched polyether modified organic silicon defoamer of nano-silica-containing, by the raw material group of following weight portion
Become：Polysiloxanes 25-40 part, hyperbranched polyether 13-23 part, allyl glycidyl ether 16-26 part, expoxy propane 38-58 part,
Bimetallic cyaniding complex 0.3-0.5 part, isopropanol 50-70 part, chloroplatinic acid catalyst 0.2-0.5 part, superfine alumina silicate 2-6
Part, D-sorbite 1-2 part, polysorbate60 1-2 part, sodium carboxymethylcellulose 2-4 part, appropriate deionized water, nano-silica powder
Last 4-11 part, dodecanol 45-60 part.
Comprise the following steps that：
（1）The preparation of end-allyl group hyperbranched polyether：
Hyperbranched polyether and bimetallic cyaniding complex are added in autoclave, vacuumize dehydration, and with nitrogen displacement 3
Secondary, after being warming up to 120 DEG C, 2/3 part of expoxy propane is passed through, controls course of reaction temperature at 130-140 DEG C or so, when pressure in kettle
During decline, allyl glycidyl ether and residual epoxide propane is added to continue polymerization a period of time, pressure no longer changes to kettle,
Vacuumize and unreacted monomer is sloughed, that is, prepare end-allyl group hyperbranched polyether；
（2）End-allyl group hyperbranched poly ether grafted polysiloxane：
Equipped with magnetic stirring apparatus, thermometer, the there-necked flask of reflux condensing tube, polysiloxanes, isopropanol and step is added
（1）The end-allyl group hyperbranched polyether of preparation, under agitation, leads to nitrogen purging 20-40 minute, adds chloroplatinic acid at 40-60 DEG C
Catalyst, under nitrogen protection, is warming up to 100-130 DEG C of reaction 3-6 hour, and vacuum distillation removes isopropanol, obtains holding allyl
Base hyperbranched poly ether grafted polysiloxane；
（3）The preparation of silicon cream：
1., nano grade silica particles are mixed with dodecanol, is placed in autoclave, be 27atm- in reaction pressure
33atm, reacts 2-4 hour under conditions of reaction temperature 200-250 DEG C, that is, obtains alcohol modified manometer silicon dioxide powder；
2., by step（2）The end-allyl group hyperbranched poly ether grafted polysiloxane for obtaining, superfine alumina silicate stirring mix 10-20
Minute, add above-mentioned alcohol modified manometer silicon dioxide powder to continue to mix afterwards, 150-170 DEG C is warming up to, insulation reaction
1-3 hour, obtains polyethers silicon cream；
（4）Add D-sorbite, polysorbate60 in deionized water, 60-90 DEG C is warming up to, stir 10-25 minute so as to completely molten
Solution, adds sodium carboxymethylcellulose afterwards, after mixing, adds above-mentioned silicon cream, quickly stirs under the conditions of 600-800r/min
50-70 minute, with high-shear emulsion machine under the conditions of 9000-10000r/min high speed shear 20-40 minute, be down to room temperature, i.e.,
Defoamer needed for obtaining.
Wherein, the hyperbranched polyether is 3- ethyl -3- methylol epoxy butane or 3- methyl -3- methylol epoxy butane
Self condense under initiator, then cation ring-opening polymerization is obtained, the degree of branching is 0.2-0.6, number-average molecular weight is 10000-
30000.
Compared with prior art, the present invention has advantages below：
（1）The present invention contains the hyperbranched polyether of great amount of hydroxy group as raw material with end, using the allyl glycidyl containing double bond structure
Epoxide group on glycerin ether occurs ring-opening polymerisation to prepare end-allyl group hyperbranched polyether with hydroxyl, using modified hyperbranched poly
There is hydrosilylation with polysiloxanes in the double bond structure of ether end group, synthesis of super branched Siloxane-Oxyalkylene Copolymers, in order to make
Standby defoamer has excellent anti-shear performance, can be suitable for multiple occasions.
（2）Hyperbranched polyether modified polyorganosiloxane prepared by the present invention is Si -- C type, and chemical stability is relatively in aqueous
Good, can preserve for a long time, while being conducive to improving its prolonged defoaming effectiveness.
（3）Little through modified nanosized silica particles size, specific surface area is big, and surface atom number is many, surface energy
It is increased dramatically with the decline of particle diameter with surface tension, and nano-silica surface there are a large amount of activity hydroxies, with chemistry
Reactivity, is combined with hyperbranched poly ether grafted polysiloxane, with obvious synergistic function, enables both preferably phases
Hold, also strengthen the two antifoam performance in high temperature environments.
Specific embodiment
A kind of hyperbranched polyether modified organic silicon defoamer of nano-silica-containing, by following weight portion（Kilogram）Original
Material composition：Polysiloxanes 35, hyperbranched polyether 22, allyl glycidyl ether 24, expoxy propane 56, bimetallic cyaniding complex
0.3, isopropanol 65, chloroplatinic acid catalyst 0.4, superfine alumina silicate 4, D-sorbite 1, polysorbate60 2, sodium carboxymethylcellulose 3,
Appropriate deionized water, nano grade silica particles 9, dodecanol 50.
Comprise the following steps that：
（1）The preparation of end-allyl group hyperbranched polyether：
Hyperbranched polyether and bimetallic cyaniding complex are added in autoclave, vacuumize dehydration, and with nitrogen displacement 3
Secondary, after being warming up to 120 DEG C, 2/3 part of expoxy propane is passed through, controls course of reaction temperature at 135 DEG C or so, when pressure drop in kettle
When, add allyl glycidyl ether and residual epoxide propane to continue polymerization a period of time, to kettle, pressure no longer changes, and takes out true
Sky sloughs unreacted monomer, that is, prepare end-allyl group hyperbranched polyether；
（2）End-allyl group hyperbranched poly ether grafted polysiloxane：
Equipped with magnetic stirring apparatus, thermometer, the there-necked flask of reflux condensing tube, polysiloxanes, isopropanol and step is added
（1）The end-allyl group hyperbranched polyether of preparation, under agitation, leads to nitrogen and purges 30 minutes, add chloroplatinic acid catalyst at 50 DEG C,
Under nitrogen protection, it is warming up to 110 DEG C to react 4 hours, vacuum distillation removes isopropanol, obtains end-allyl group hyperbranched polyether and connects
Branch polysiloxanes；
（3）The preparation of silicon cream：
1., nano grade silica particles are mixed with dodecanol, is placed in autoclave, be 30atm in reaction pressure, instead
React 3 hours under conditions of answering 230 DEG C of temperature, that is, obtain alcohol modified manometer silicon dioxide powder；
2., by step（2）The end-allyl group hyperbranched poly ether grafted polysiloxane for obtaining, superfine alumina silicate stirring mix 15 points
Clock, adds above-mentioned alcohol modified manometer silicon dioxide powder to continue to mix afterwards, is warming up to 160 DEG C, insulation reaction 2 hours,
Obtain polyethers silicon cream；
（4）Add D-sorbite, polysorbate60 in deionized water, 80 DEG C are warming up to, stir 20 minutes so as to be completely dissolved, it
Add sodium carboxymethylcellulose afterwards, after mixing, above-mentioned silicon cream is added, quick stirring 60 minutes, use under the conditions of 800r/min
High-shear emulsion machine high speed shear 30 minutes under the conditions of 9000r/min, are down to room temperature, obtain final product required defoamer.
Wherein, the hyperbranched polyether is 3- ethyl -3- methylol epoxy butane or 3- methyl -3- methylol epoxy butane
Self condense under initiator, then cation ring-opening polymerization is obtained, the degree of branching is 0.5, number-average molecular weight is 20000.
The antifoam performance of defoamer of the present invention is evaluated with Bubbling method：
At 85-150 DEG C, basicity>In the bubbling system of 10mg/L, antifoam performance is less than 110mm foam height, and suds suppressing properties are less than
220mm foam height.
Claims (3)
1. the hyperbranched polyether modified organic silicon defoamer of a kind of nano-silica-containing, it is characterised in that by following weight portion
Raw material composition：Polysiloxanes 25-40 part, hyperbranched polyether 13-23 part, allyl glycidyl ether 16-26 part, expoxy propane
38-58 part, bimetallic cyaniding complex 0.3-0.5 part, isopropanol 50-70 part, chloroplatinic acid catalyst 0.2-0.5 part, ultra-fine silicon
Sour aluminium 2-6 part, D-sorbite 1-2 part, polysorbate60 1-2 part, sodium carboxymethylcellulose 2-4 part, appropriate deionized water, nanometer two
Silicon oxide powder 4-11 part, dodecanol 45-60 part.
2. the system of the hyperbranched polyether modified organic silicon defoamer of a kind of nano-silica-containing according to claims 1
Preparation Method, it is characterised in that comprise the following steps that：
（1）The preparation of end-allyl group hyperbranched polyether：
Hyperbranched polyether and bimetallic cyaniding complex are added in autoclave, vacuumize dehydration, and with nitrogen displacement 3
Secondary, after being warming up to 120 DEG C, 2/3 part of expoxy propane is passed through, controls course of reaction temperature at 130-140 DEG C or so, when pressure in kettle
During decline, allyl glycidyl ether and residual epoxide propane is added to continue polymerization a period of time, pressure no longer changes to kettle,
Vacuumize and unreacted monomer is sloughed, that is, prepare end-allyl group hyperbranched polyether；
（2）End-allyl group hyperbranched poly ether grafted polysiloxane：
Equipped with magnetic stirring apparatus, thermometer, the there-necked flask of reflux condensing tube, polysiloxanes, isopropanol and step is added
（1）The end-allyl group hyperbranched polyether of preparation, under agitation, leads to nitrogen purging 20-40 minute, adds chloroplatinic acid at 40-60 DEG C
Catalyst, under nitrogen protection, is warming up to 100-130 DEG C of reaction 3-6 hour, and vacuum distillation removes isopropanol, obtains holding allyl
Base hyperbranched poly ether grafted polysiloxane；
（3）The preparation of silicon cream：
1., nano grade silica particles are mixed with dodecanol, is placed in autoclave, be 27atm- in reaction pressure
33atm, reacts 2-4 hour under conditions of reaction temperature 200-250 DEG C, that is, obtains alcohol modified manometer silicon dioxide powder；
2., by step（2）The end-allyl group hyperbranched poly ether grafted polysiloxane for obtaining, superfine alumina silicate stirring mix 10-20
Minute, add above-mentioned alcohol modified manometer silicon dioxide powder to continue to mix afterwards, 150-170 DEG C is warming up to, insulation reaction
1-3 hour, obtains polyethers silicon cream；
（4）Add D-sorbite, polysorbate60 in deionized water, 60-90 DEG C is warming up to, stir 10-25 minute so as to completely molten
Solution, adds sodium carboxymethylcellulose afterwards, after mixing, adds above-mentioned silicon cream, quickly stirs under the conditions of 600-800r/min
50-70 minute, with high-shear emulsion machine under the conditions of 9000-10000r/min high speed shear 20-40 minute, be down to room temperature, i.e.,
Defoamer needed for obtaining.
3. the hyperbranched polyether modified organic silicon defoamer of a kind of nano-silica-containing according to claims 1,2
Preparation method, it is characterised in that the hyperbranched polyether is 3- ethyl -3- methylol epoxy butane or 3- methyl -3- methylol
Epoxy butane is self condensed under initiator, and then cation ring-opening polymerization is obtained, and the degree of branching is 0.2-0.6, and number-average molecular weight is
10000-30000.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107603704A (en) * | 2017-09-17 | 2018-01-19 | 刘翠芬 | Aqueous release agent for clear-water concrete and preparation method thereof |
| CN110743208A (en) * | 2019-09-09 | 2020-02-04 | 西安理工大学 | Nano defoaming agent and preparation method and application thereof |
| CN111744236A (en) * | 2020-08-14 | 2020-10-09 | 杭州富阳诚科通信材料有限公司 | Polyether modified organic silicon defoaming agent and preparation method thereof |
| CN112295270A (en) * | 2020-10-11 | 2021-02-02 | 金华市铨沥科技有限公司 | Preparation method of defoaming agent for fermentation production of epothilone |
| CN115193105A (en) * | 2022-07-21 | 2022-10-18 | 威尔（福建）生物有限公司 | Defoaming agent for papermaking white water and preparation method thereof |
| CN115228148A (en) * | 2022-09-26 | 2022-10-25 | 烟台恒鑫化工科技有限公司 | Composite defoaming agent for oil field and preparation method thereof |
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Cited By (9)
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|---|---|---|---|---|
| CN107603704A (en) * | 2017-09-17 | 2018-01-19 | 刘翠芬 | Aqueous release agent for clear-water concrete and preparation method thereof |
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| CN111744236A (en) * | 2020-08-14 | 2020-10-09 | 杭州富阳诚科通信材料有限公司 | Polyether modified organic silicon defoaming agent and preparation method thereof |
| CN112295270A (en) * | 2020-10-11 | 2021-02-02 | 金华市铨沥科技有限公司 | Preparation method of defoaming agent for fermentation production of epothilone |
| CN115193105A (en) * | 2022-07-21 | 2022-10-18 | 威尔（福建）生物有限公司 | Defoaming agent for papermaking white water and preparation method thereof |
| CN115193105B (en) * | 2022-07-21 | 2024-04-12 | 威尔（福建）生物有限公司 | Defoaming agent for papermaking white water and preparation method thereof |
| CN115228148A (en) * | 2022-09-26 | 2022-10-25 | 烟台恒鑫化工科技有限公司 | Composite defoaming agent for oil field and preparation method thereof |
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