CN106390532A - High-temperature-resistant and alkali-resistant hyperbranched polyether modified organic silicon defoamer and preparation method thereof - Google Patents
High-temperature-resistant and alkali-resistant hyperbranched polyether modified organic silicon defoamer and preparation method thereof Download PDFInfo
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- CN106390532A CN106390532A CN201610904641.9A CN201610904641A CN106390532A CN 106390532 A CN106390532 A CN 106390532A CN 201610904641 A CN201610904641 A CN 201610904641A CN 106390532 A CN106390532 A CN 106390532A
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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
- B01D19/0431—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance containing aromatic rings
- B01D19/0436—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance containing aromatic rings with substituted groups
- B01D19/0454—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance containing aromatic rings with substituted groups which contain S-atoms
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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
- C08G81/00—Macromolecular compounds obtained by interreacting polymers in the absence of monomers, e.g. block polymers
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Abstract
The invention discloses a high-temperature-resistant and alkali-resistant hyperbranched polyether modified organic silicon defoamer. The defoamer is prepared from raw materials in parts by weight as follows: 25-40 parts of polysiloxane, 16-24 parts of hyperbranched polyether, 17-25 parts of allyl glycidyl ether, 42-57 parts of propylene oxide, 0.3-0.5 parts of a bimetal cyanided complex, 50-70 parts of isopropyl alcohol, 0.2-0.6 parts of a chloroplatinic acid catalyst, 3-6 parts of superfine aluminum silicate, 1-2 parts of sorbitol, 1-2 parts of Tween 60, 2-4 parts of sodium carboxymethyl cellulose, a proper amount of deionized water, 1-3 parts of wollastonite, 2-3 parts of nano silicon oxide and 3-5 parts of sodium p-styrene sulfonate. Hyperbranched polyether containing a lot of hydroxyl groups at tail ends is used as the raw material, allyl-terminated hyperbranched polyether is prepared, a modified hyperbranched polyether-terminated double bond structure and polysiloxane are subjected to a hydrosilylation reaction, hyperbranched polyether modified polysiloxane is synthesized, and the defoamer prepared from the hyperbranched polyether modified polysiloxane has excellent shear resistance.
Description
Technical field
The present invention relates to chemicals field, more particularly to a kind of high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon disappears
Infusion and preparation method thereof.
Technical background
Defoamer, is also called defrother or foamicide, can produce the bubble that many impacts produce during commercial production
Foam, needs to add defoamer.It is widely used in removing latex, textile sizing, food fermentation, biological medicine, coating, oil
The unwanted bubbles producing during the industry production such as work, papermaking, industry cleaning link, sewage disposal.
Existing defoamer can be divided into organic silicon type and polyether-type two big class according to composition, and organic silicon defoamer is due to emulsifying
The addition of the auxiliary agents such as agent, easily 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 is 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 suitability of exploitation in recent years, the research layer of the higher defoamer of defoaming effectiveness
Go out not poor.Polyether modified polysiloxan defoaming agent is passed through to introduce polyether segment on silicone oil segment, thus it is common to have two kinds of defoamer concurrently
Advantage, froth breaking effect is strong, and thermostability, shear resistant and acid-proof alkaline are good.But the polyether modified silicon oil of current research disappears
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 macromole that a class has torispherical structure, containing a large amount of functional end-groups,
There is low melt and solution viscosity.After linear polymer is sheared, molecular backbone is interrupted, lead to molecular weight significantly under
Fall, and after dissaving polymer is sheared, only can interrupt a certain branched structure, do 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 it《The synthesis of water solublity high shear hyperbranched poly acrylamide and sign》
In one literary composition, raw radical polymerization is issued in cerium salt-hydroxyl initiator system with hyperbranched polyglycidyl ether, acrylamide, obtains
Highly branched water-soluble ultrabranching polyacrylamide HPG-star-PAM, 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 high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon froth breaking
Agent and preparation method thereof.
A kind of high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon defoamer, is made up of the raw material of following weight portion：Poly-
Siloxanes 25-40 part, hyperbranched polyether 16-24 part, allyl glycidyl ether 17-25 part, expoxy propane 42-57 part, double gold
Belong to cyanide complex 0.3-0.5 part, isopropanol 50-70 part, chloroplatinic acid catalyst 0.2-0.6 part, superfine alumina silicate 3-6 part, mountain
Pears sugar alcohol 1-2 part, polysorbate60 1-2 part, sodium carboxymethyl cellulose 2-4 part, appropriate deionized water, wollastonite 1-3 part, nano oxygen
SiClx 2-3 part, sodium p styrene sulfonate 3-5 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, evacuation is dehydrated, and with nitrogen displacement 3
Secondary, after being warming up to 120 DEG C, it is passed through 2/3 part of expoxy propane, control course of reaction temperature at 130-140 DEG C about, 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,
Evacuation sloughs unreacted monomer, that is, prepare end-allyl group hyperbranched polyether；
（2）End-allyl group hyperbranched poly ether grafted polysiloxane：
Equipped with magnetic stirring apparatuss, thermometer, the there-necked flask of reflux condensing tube, add polysiloxanes, isopropanol and step
（1）The end-allyl group hyperbranched polyether of preparation, under agitation, at 40-60 DEG C, logical nitrogen purging 20-40 minute, adds chloroplatinic acid
Catalyst, under nitrogen protection, is warming up to 100-130 DEG C of reaction 3-6 hour, vacuum distillation removes isopropanol, obtains holding allyl
Base hyperbranched poly ether grafted polysiloxane；
（3）By step（2）The end-allyl group hyperbranched poly ether grafted polysiloxane obtaining is uniformly mixed with superfine alumina silicate,
It is warming up to 150-170 DEG C, insulation reaction 1-3 hour, obtain polyethers silicon cream；
（4）By nano silicon oxide, wollastonite and deionized water mix homogeneously, under the power of 1000W, ultrasonic 1-2 hour, is mixed
Close dispersion liquid, standby；
（5）Add Sorbitol, polysorbate60 in deionized water, be warming up to 60-90 DEG C, stirring 10-25 minute is so as to completely molten
Solution, adds sodium carboxymethyl cellulose afterwards, after mix homogeneously, adds above-mentioned silicon cream, quickly stirs under the conditions of 600-800r/min
50-70 minute, adds sodium p styrene sulfonate, step afterwards（4）The mixed dispersion liquid obtaining, is existed with high-shear emulsion machine
High speed shear 20-40 minute under the conditions of 9000-10000r/min, is down to room temperature, obtains final product required defoamer.
Wherein, described 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 obtains, 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 and hydroxyl occur ring-opening polymerisation to prepare end-allyl group hyperbranched polyether, 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）The hyperbranched polyether modified polyorganosiloxane of present invention preparation is Si -- C type, and chemical stability is relatively in aqueous
Good, can preserve for a long time, be conducive to improving its long defoaming effectiveness simultaneously.
（3）The present invention adopts wollastonite as carrier, adds sodium p styrene sulfonate to make this defoamer and foam system
Preferably combine, substantially increase the performance of defoamer, and its stability is good, remain to keep good in high temperature and strong alkali environment
Good antifoaming performance and stability.
Specific embodiment
A kind of high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon defoamer, by following weight portion（Kilogram）Raw material group
Become：Polysiloxanes 36, hyperbranched polyether 21, allyl glycidyl ether 23, expoxy propane 55, bimetallic cyaniding complex 0.4,
Isopropanol 65, chloroplatinic acid catalyst 0.4, superfine alumina silicate 4, Sorbitol 2, polysorbate60 1, sodium carboxymethyl cellulose 3, go from
Sub- appropriate amount of water, wollastonite 3, nano silicon oxide 2, sodium p styrene sulfonate 4.
Comprise the following steps that：
（1）The preparation of end-allyl group hyperbranched polyether：
Hyperbranched polyether and bimetallic cyaniding complex are added in autoclave, evacuation is dehydrated, and with nitrogen displacement 3
Secondary, after being warming up to 120 DEG C, it is passed through 2/3 part of expoxy propane, control course of reaction temperature at 135 DEG C about, when pressure drop in kettle
When, add allyl glycidyl ether and residual epoxide propane to continue polymerization a period of time, pressure no longer changes to kettle, 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 apparatuss, thermometer, the there-necked flask of reflux condensing tube, add polysiloxanes, isopropanol and step
（1）The end-allyl group hyperbranched polyether of preparation, under agitation, at 50 DEG C, logical nitrogen purges 30 minutes, adds chloroplatinic acid catalyst,
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）By step（2）The end-allyl group hyperbranched poly ether grafted polysiloxane obtaining is uniformly mixed with superfine alumina silicate,
It is warming up to 160 DEG C, insulation reaction 2 hours, obtain polyethers silicon cream；
（4）By nano silicon oxide, wollastonite and deionized water mix homogeneously, ultrasonic 2 hours under the power of 1000W, mixed
Dispersion liquid, standby；
（5）Add Sorbitol, polysorbate60 in deionized water, be warming up to 80 DEG C, stir 20 minutes so as to be completely dissolved, it
Add sodium carboxymethyl cellulose afterwards, after mix homogeneously, add above-mentioned silicon cream, quick stirring 60 minutes under the conditions of 800r/min, it
Add sodium p styrene sulfonate, step afterwards（4）The mixed dispersion liquid obtaining, with high-shear emulsion machine under the conditions of 9000r/min
High speed shear 30 minutes, is down to room temperature, obtains final product required defoamer.
Wherein, described 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 obtains, the degree of branching is 0.5, number-average molecular weight is 20000.
The antifoam performance Bubbling method of defoamer of the present invention is evaluated：
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. a kind of high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon defoamer is it is characterised in that former by following weight portion
Material composition：Polysiloxanes 25-40 part, hyperbranched polyether 16-24 part, allyl glycidyl ether 17-25 part, expoxy propane 42-
57 parts, bimetallic cyaniding complex 0.3-0.5 part, isopropanol 50-70 part, chloroplatinic acid catalyst 0.2-0.6 part, superfine alumina silicate
3-6 part, Sorbitol 1-2 part, polysorbate60 1-2 part, sodium carboxymethyl cellulose 2-4 part, appropriate deionized water, wollastonite 1-3
Part, nano silicon oxide 2-3 part, sodium p styrene sulfonate 3-5 part.
2. the preparation side of a kind of high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon defoamer according to claims 1
Method is 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, evacuation is dehydrated, and with nitrogen displacement 3
Secondary, after being warming up to 120 DEG C, it is passed through 2/3 part of expoxy propane, control course of reaction temperature at 130-140 DEG C about, 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,
Evacuation sloughs unreacted monomer, that is, prepare end-allyl group hyperbranched polyether；
（2）End-allyl group hyperbranched poly ether grafted polysiloxane：
Equipped with magnetic stirring apparatuss, thermometer, the there-necked flask of reflux condensing tube, add polysiloxanes, isopropanol and step
（1）The end-allyl group hyperbranched polyether of preparation, under agitation, at 40-60 DEG C, logical nitrogen purging 20-40 minute, adds chloroplatinic acid
Catalyst, under nitrogen protection, is warming up to 100-130 DEG C of reaction 3-6 hour, vacuum distillation removes isopropanol, obtains holding allyl
Base hyperbranched poly ether grafted polysiloxane；
（3）By step（2）The end-allyl group hyperbranched poly ether grafted polysiloxane obtaining is uniformly mixed with superfine alumina silicate,
It is warming up to 150-170 DEG C, insulation reaction 1-3 hour, obtain polyethers silicon cream；
（4）By nano silicon oxide, wollastonite and deionized water mix homogeneously, under the power of 1000W, ultrasonic 1-2 hour, is mixed
Close dispersion liquid, standby；
（5）Add Sorbitol, polysorbate60 in deionized water, be warming up to 60-90 DEG C, stirring 10-25 minute is so as to completely molten
Solution, adds sodium carboxymethyl cellulose afterwards, after mix homogeneously, adds above-mentioned silicon cream, quickly stirs under the conditions of 600-800r/min
50-70 minute, adds sodium p styrene sulfonate, step afterwards（4）The mixed dispersion liquid obtaining, is existed with high-shear emulsion machine
High speed shear 20-40 minute under the conditions of 9000-10000r/min, is down to room temperature, obtains final product required defoamer.
3. the preparation of a kind of high temperature resistant alkaline-resisting hyperbranched polyether modified organic silicon defoamer according to claims 1,2
Method is it is characterised in that described hyperbranched polyether is 3- ethyl -3- methylol epoxy butane or 3- methyl -3- methylol epoxy
Butane self condenses under initiator, and then cation ring-opening polymerization obtains, and the degree of branching is 0.2-0.6, and number-average molecular weight is
10000-30000.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743208A (en) * | 2019-09-09 | 2020-02-04 | 西安理工大学 | Nano defoaming agent and preparation method and application thereof |
| CN113416593A (en) * | 2021-06-18 | 2021-09-21 | 安徽博洋润滑科技有限公司 | Long-life extreme pressure antiwear hydraulic oil and preparation method thereof |
| CN114316609A (en) * | 2021-09-03 | 2022-04-12 | 南京瑞思化学技术有限公司 | Preparation method of silicon ether composition |
| CN115286800A (en) * | 2022-08-26 | 2022-11-04 | 南京瑞思化学技术有限公司 | Preparation method of hyperbranched organic silicon emulsifier |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891894A (en) * | 2008-10-29 | 2010-11-24 | 赢创戈尔德施米特有限公司 | Silicone-polyether copolymer systems and process for preparing them by means of an alkoxylation reaction |
| CN103768834A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Defoaming agent composition |
-
2016
- 2016-10-18 CN CN201610904641.9A patent/CN106390532A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101891894A (en) * | 2008-10-29 | 2010-11-24 | 赢创戈尔德施米特有限公司 | Silicone-polyether copolymer systems and process for preparing them by means of an alkoxylation reaction |
| CN103768834A (en) * | 2012-10-24 | 2014-05-07 | 中国石油化工股份有限公司 | Defoaming agent composition |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110743208A (en) * | 2019-09-09 | 2020-02-04 | 西安理工大学 | Nano defoaming agent and preparation method and application thereof |
| CN110743208B (en) * | 2019-09-09 | 2021-08-06 | 西安理工大学 | Nano defoaming agent and preparation method and application thereof |
| CN113416593A (en) * | 2021-06-18 | 2021-09-21 | 安徽博洋润滑科技有限公司 | Long-life extreme pressure antiwear hydraulic oil and preparation method thereof |
| CN114316609A (en) * | 2021-09-03 | 2022-04-12 | 南京瑞思化学技术有限公司 | Preparation method of silicon ether composition |
| CN115286800A (en) * | 2022-08-26 | 2022-11-04 | 南京瑞思化学技术有限公司 | Preparation method of hyperbranched organic silicon emulsifier |
| CN115286800B (en) * | 2022-08-26 | 2023-03-28 | 南京瑞思化学技术有限公司 | Preparation method of hyperbranched organic silicon emulsifier |
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Application publication date: 20170215 |