CN106215467A - A kind of organic silicon defoamer - Google Patents
A kind of organic silicon defoamer Download PDFInfo
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- CN106215467A CN106215467A CN201610742713.4A CN201610742713A CN106215467A CN 106215467 A CN106215467 A CN 106215467A CN 201610742713 A CN201610742713 A CN 201610742713A CN 106215467 A CN106215467 A CN 106215467A
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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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Abstract
The present invention relates to a kind of froth breaking suds product be applicable to chemical industry, be specifically related to a kind of organic silicon defoamer.It is made up of the water of the silicon composition A of 5～30 parts, the polyether-modified polysiloxane B of 10～30 parts, the emulsifying agent C of 2～10 parts, the coupling agent D of 0.01～0.1 part, the thickening agent E of 2～10 parts and 30～60 parts；Coupling agent D is selected from MTMS, MTES, amino trimethoxy silane or amino triethoxysilane.The organic silicon defoamer of the present invention, significantly improves emulsion intercalation method so that it is have preferable stability in the extreme condition such as strong acid, highly basic, improves the persistency of defoamer, should not separate out simultaneously.
Description
Technical field
The present invention relates to a kind of froth breaking suds product be applicable to chemical industry, be specifically related to a kind of organosilicon froth breaking
Agent.
Background technology
Defoamer, also referred to as anti-foam agent, be reduction surface tension in the course of processing, and suppression foam produces or eliminates and produces
Foam.China is permitted spendable defoamer the fatty acid ester compounded thing of organosilicon emulsion-type, higher alcohols, polyoxyethylene polyoxypropylene
Tetramethylolmethane ether, polyoxyethylene polyoxy propanol amidogen ether, polypropylene glycerol aether and polyoxyethylene polyoxypropylene glycerin ether, poly-diformazan
Radical siloxane etc..Organosilicon emulsion-type defoamer is very fast due to froth breaking, is widely used in industrialized production, but, due to breast
Liquid is a meta system, the phenomenon such as breakdown of emulsion, layering often occurs, have a strong impact on product matter during transport and use
The most how amount, improve the stability of emulsion of defoamer, all the time, be all that defoamer preparation manufacturer technology to be solved is difficult
Topic.
CN101003008B provides a kind of method improving stability of emulsion, mainly by containing as emulsifying agent
The pfpe molecule having hydroxyl is modified, and uses the emulsifying agent with closed-end structure to carry out high fatty alcohol, higher fatty acids
Emulsion, the emulsion obtained has heat resistance and anti-shear performance.But and the emulsifying agent of undeclared this modification is to organosilicon
The effectiveness of class defoamer.EP0341952 is to use compounding to polysiloxane and Siloxane-Oxyalkylene Copolymers, carries further
The antifoaming performance of high emulsion.But still the problem of the easy chain rupture of siloxanes in strong acid-base system can not be solved, at highly basic body
In system poor for applicability.Patent CN103074784 provides a kind of method using starch as stabilizer and improves emulsion resistance to acids and bases
Can, but owing to stabilizing agent dosage is bigger so that antifoaming performance is deteriorated.CN103603215A provides a kind of acid and alkali-resistance system
The preparation method of organic silicon defoamer, mainly compare the addition sequence of hydrophilic, oleophilic emulsifier to stability of emulsion and
The impact of resistance to acids and bases, by by after oleophilic emulsifier and silicon composition elder generation mixing and stirring, adding hydrophilic emulsifying
Agent can improve stability of emulsion and resistance to acids and bases, but this technique can not the most effectively solve resistance to acids and bases
Problem.US005773407A is after defoamer emulsion prepares, and adds alkylalkoxy silane and catalyst reaction, is formed
A kind of to defoamer emulsion particle protective layer, improve stability, especially improve the compatibility in liquid detergent.
Summary of the invention
For above deficiency, it is an object of the invention to provide a kind of organic silicon defoamer, be remarkably improved emulsion
Stability so that it is have preferable stability in the extreme condition such as strong acid, highly basic, improves the persistency of defoamer, simultaneously
Should not separate out.
For achieving the above object, present invention employs techniques below scheme:
A kind of organic silicon defoamer, according to weight portion meter, is made up of following raw material:
The silicon composition A of 5～30 parts, the polyether-modified polysiloxane B of 10～30 parts, the emulsifying of 2～10 parts
Agent C, the coupling agent D of 0.01～0.1 part, the thickening agent E of 2～10 parts, the water of 30～60 parts；Coupling agent D is selected from methyl trimethoxy oxygen
Base silane, MTES, amino trimethoxy silane or amino triethoxysilane；
The preparation method of organic silicon defoamer is:
(1), by silicon composition A, polyether-modified polysiloxane B and emulsifying agent C mix, then heat to 50～
80 DEG C, stirring 0.5～1.5h, speed of agitator is 100～400rpm；
(2), keep temperature-resistant, while stirring addition 30～the thickening agent E of the water of 60%, 70～90% and coupling agent
D, regulates pH to 6.5～7.0；
(3), above-mentioned emulsion is homogenized by colloid mill, and the thickening agent E and water dilution by surplus is disappeared
Infusion.
Described polyether-modified polysiloxane B is to be reacted by containing hydrogen silicone oil and unsaturated polyether to prepare, preparation process
Middle selection chloroplatinic acid is as catalyst, and reaction temperature is 80～200 DEG C.The structural formula of described polyether-modified polysiloxane B
For:
MDa(MeYSiO)bM
Wherein, M is chain link R3SiO1/2, D is chain link R2SiO2/2, R is identical or different, selected from hydrogen atom, the replacement of monovalence or
Non-substituted carbon number is the alkyl of 1～20；Me is methyl；The structural formula of Y is :-(CH2)zO(EO)g(PO)hK, K are end-blocking
Group, selected from hydrogen atom, methyl, ethyl, propyl group, butyl；Subscript a, b, z, g, h are the degree of polymerization, and a is the integer of 10～500, b
Being the integer of 1～50, z is the integer of 2～6, and g is the integer of 1～36, and h is the integer of 0～20.The present invention selects HLB value to be 10
～the Siloxane-Oxyalkylene Copolymers of 20, its dynamic viscosity when 25 DEG C is 200～2000mPa s.
Described emulsifying agent C is nonionic surfactant or anion surfactant, mainly has alkylphenol-polyethenoxy
Ether (includes NPE, OPEO, dodecyl phenol polyethenoxy ether and binonylphenol polyoxy second
Alkene ether), aliphatic acid polyethenoxy ether (include lauric acid polyoxyethylene ether, oleic acid polyoxyethylene, Palmic acid polyoxyethylene ether,
Stearic acid polyoxyethylene ether), fatty alcohol-polyoxyethylene ether, Sorbitan alcohol ether stearate polyoxyethylene ether, Oleum Ricini polyoxy
Vinyl Ether.
Described thickening agent E is selected from polyacrylamide, carbomer, HANSHENGJIAO, cellulose or polyacrylic acid.
Described silicon composition A uses polysiloxane A (1) and A (2), silicon dioxide A (3), organic siliconresin A
(4) prepare with catalyst A (5)；
A (1) polysiloxane:
At least one general structure is RaSiO4-a/2Polysiloxane:
Wherein the value of a is 1.9～2.2, and the substituent R in molecular structure is identical or different, and including hydrogen atom, carbon is former
Subnumber is the alkyl of 1～20, preferably methyl.The polysiloxane A (1) that the present invention uses is the poly-of trimethylsiloxy group end-blocking
Dimethyl siloxane, this polysiloxane dynamic viscosity when 25 DEG C is 1000～300000mPa.s；A (1) is poly-organic
Siloxanes occupies 10～60 parts at silicon composition A.
A (2) polysiloxane:
At least one has general structure is R2 b(R1O)cSiO(4-b-c)/2Polysiloxane:
Wherein b is 0,1,2 or 3, and c is 1,2 or 3, b+c≤3, all of R in molecular structure1Identical or different, R2Identical
Or different, R1And R2Value consistent with the R that A (1) plants.The polysiloxane A (2) that the present invention uses is hydroxy-end capped gathering
Dimethyl siloxane, this polysiloxane dynamic viscosity when 25 DEG C is 1000～200000mPa.s；A (2) is poly-organic
Siloxanes occupies 40～90 parts at silicon composition A.
A (3) silicon dioxide
Described silicon dioxide includes aerosil or precipitated silica, and specific surface area is 50～500m2/ g, can
With pass through or process without hydrophobization.The preferred specific surface area of the present invention is 90～300m2The precipitated silica of/g or gas
Aerosil.A (3) silicon dioxide occupies 5 parts at silicon composition A.
A (4) organic siliconresin
Described organic siliconresin refers to the polysiloxane of highly cross-linked space net structure, this cancellated
Polysiloxane be typically by methyl trichlorosilane, dimethyldichlorosilane, phenyl trichlorosilane, diphenyl dichlorosilane or
The various mixture of dichloromethyl phenylsilane hydrolyze in organic solvent is such as toluene, obtain acidic hydrolysis thing, then through washing
Remove acid, obtain product.The organic siliconresin that the present invention uses is by chain link CH3SiO1/2(organosilicon chemistry is referred to as M unit)
With chain link SiO4/2The MQ resin of the unit composition of (Q unit), mol ratio therebetween is (0.4～1.2): 1.0, preferably
(0.5～0.8): 1.0.A (4) organic siliconresin occupies 10 parts at silicon composition A.
A (5) catalyst
Described catalyst is used to accelerate reaction between coupling agent and polysiloxane.Including alkali metal hydroxide
Thing, alkali metal silane alkoxide, alkali metal alkoxide, the hydroxide of quaternary ammonium salt, refer specifically to sodium hydroxide, potassium hydroxide,
Cesium hydrate., methyl silanol potassium, methyl silicon sodium alcoholate, Feldalat NM, Sodium ethylate, Feldalat KM, potassium ethoxide, beta-hydroxyethyl trimethyl ammonium,
Tetramethylammonium hydroxide etc., preferably potassium hydroxide.A (5) catalyst occupies 0.1～5 part at silicon composition A.
The preparation method of described silicon composition A is: by polysiloxane A (1), A (2) and organic siliconresin A (4)
In stirrer for mixing, it is warming up to 40～140 DEG C, adds catalyst A (5), polyreaction occurs；When mixing reaches certain viscosity
Rear addition, as the silicon dioxide A (3) of water repellent agent, is reacted 1～7h at 60～140 DEG C, is the most further warming up to
160～230 DEG C, react 1～4h；After completion of the reaction, under-0.01～-0.08MPa vacuum, maintenance 0.1～0.5h, the coldest
But arrive room temperature, obtain silicon composition A.
There is hydrolysis in alkoxy silane, the hydroxyl after hydrolysis can be condensed into netted in the periphery of silicon composition
Structure, can form hydrogen bond with the hydroxyl in silicon composition simultaneously, play the effect of protection silicon composition, thus aobvious
Write and improve emulsion intercalation method so that it is there is in the extreme condition such as strong acid, highly basic preferable stability, improve defoamer
Persistency, should not separate out simultaneously.It is applied in the degreasing agent of alkali system, it is possible to keep preferable defoaming and suds
Property, be conducive to cleaning to produce and save the energy.Defoamer product emulsion prepared by the present invention, can be used for tool in metal cleaning industry
Have in the degreasing agent of alkali system, improve defoamer stability in alkali system, improve suds suppressing properties.
Detailed description of the invention
Below with reference to embodiment, the present invention is described in detail.But, embodiment content is only to this
Bright example and explanation, described specific embodiment is done various repairing by affiliated those skilled in the art
Change or supplement or use similar mode to substitute, without departing from the design of invention or surmount defined in the claims
Scope, all should belong to protection scope of the present invention.
The preparation of silicon composition A:
By polysiloxane A (1), A (2) and organic siliconresin A (4) in stirrer for mixing, it is warming up to 100 DEG C, adds
Enter catalyst A (5), polyreaction occurs；The silicon dioxide A as water repellent agent is added after mixing reaches certain viscosity
(3), at 80 DEG C, react 5h, be the most further warming up to 200 DEG C, react 2h；After completion of the reaction, in-0.01MPa vacuum
Lower maintenance 0.3h, is finally cooled to room temperature, obtains silicon composition A.
Wherein:
A (1) polysiloxane:
Polysiloxane A (1) is the polydimethylsiloxane of trimethylsiloxy group end-blocking, and this polysiloxane is 25
DEG C time dynamic viscosity be 1000～300000mPa.s；A (1) polysiloxane occupies 20 parts at silicon composition A.
A (2) polysiloxane:
Polysiloxane A (2) is hydroxy-end capped polydimethylsiloxane, this polysiloxane moving when 25 DEG C
Mechanics viscosity is 1000～200000mPa.s；A (2) polysiloxane occupies 50 parts at silicon composition A.
A (3) silicon dioxide
Silicon dioxide specific surface area is 200m2The precipitated silica of/g.A (3) silicon dioxide accounts at silicon composition A
There are 5 parts.
A (4) organic siliconresin
Organic siliconresin is by chain link CH3SiO1/2(M unit) and chain link SiO4/2The MQ tree of the unit composition of (Q unit)
Fat, mol ratio therebetween is 0.8:1.0.A (4) organic siliconresin occupies 10 parts at silicon composition A.
A (5) catalyst
Catalyst is potassium hydroxide.A (5) catalyst occupies 0.8 part at silicon composition A.
The preparation of polyether-modified polysiloxane B:
Polyether-modified polysiloxane B is to be reacted by containing hydrogen silicone oil and unsaturated polyether to prepare, and selects in preparation process
With chloroplatinic acid as catalyst, reaction temperature is 120 DEG C.The structural formula of described polyether-modified polysiloxane B is:
MDa(MeYSiO)bM
Wherein, M is chain link R3SiO1/2, D is chain link R2SiO2/2, R is identical selected from hydrogen atom；Me is methyl；The structural formula of Y
For :-(CH2)zO(EO)g(PO)hK, K are end-capping group, selected from hydrogen atom；Subscript a, b, z, g, h are the degree of polymerization, and a is 50, and b is
25, z is 4, and g is 20, and h is 5.
Embodiment 1
A kind of organic silicon defoamer, according to weight portion meter, is made up of following raw material:
The silicon composition A of 5 parts, the polyether-modified polysiloxane B of 30 parts, 2 parts emulsifying agent C (nonyl phenol gather
Oxygen vinyl Ether), the coupling agent D (MTMS) of 0.1 part, the thickening agent E (polyacrylic acid) of 2 parts, the water of 60 parts.
The preparation method of organic silicon defoamer is:
(1), silicon composition A, polyether-modified polysiloxane B and emulsifying agent C are mixed, then heat to 50
DEG C, stirring 1.5h, speed of agitator is 100rpm；
(2), keep temperature-resistant, add water, the thickening agent E and coupling agent D of 70% of 60% while stirring, regulate pH
To 7.0；
(3), above-mentioned emulsion is homogenized by colloid mill, and the thickening agent E and water dilution by surplus is disappeared
Infusion.
Embodiment 2
A kind of organic silicon defoamer, according to weight portion meter, is made up of following raw material:
The silicon composition A of 30 parts, the polyether-modified polysiloxane B of 10 parts, the emulsifying agent C (Palmic acid of 10 parts
Polyoxyethylene ether), the coupling agent D (MTES) of 0.01 part, the thickening agent E (carbomer) of 10 parts, the water of 30 parts.
The preparation method of organic silicon defoamer is:
(1), silicon composition A, polyether-modified polysiloxane B and emulsifying agent C are mixed, then heat to 80
DEG C, stirring 0.5h, speed of agitator is 400rpm；
(2), keep temperature-resistant, add water, the thickening agent E and coupling agent D of 90% of 30% while stirring, regulate pH
To 6.5；
(3), above-mentioned emulsion is homogenized by colloid mill, and the thickening agent E and water dilution by surplus is disappeared
Infusion.
Embodiment 3
A kind of organic silicon defoamer, according to weight portion meter, is made up of following raw material:
The silicon composition A of 25 parts, the polyether-modified polysiloxane B of 20 parts, the emulsifying agent C (Sorbitan of 5 parts
Alcohol ether stearate polyoxyethylene ether), the coupling agent D (amino trimethoxy silane) of 0.05 part, the thickening agent E (polypropylene of 5 parts
Amide), the water of 45 parts.
The preparation method of organic silicon defoamer is:
(1), silicon composition A, polyether-modified polysiloxane B and emulsifying agent C are mixed, then heat to 65
DEG C, stirring 1h, speed of agitator is 250rpm；
(2), keep temperature-resistant, add water, the thickening agent E and coupling agent D of 80% of 45% while stirring, regulate pH
To 6.8；
(3), above-mentioned emulsion is homogenized by colloid mill, and the thickening agent E and water dilution by surplus is disappeared
Infusion.
Comparative example 1
And differing only in without component D between embodiment 1, other components and preparation method are identical.
Comparative example 2
And differing only in without component D between embodiment 2, other components and preparation method are identical.
Comparative example 3
And differing only in without component D between embodiment 3, other components and preparation method are identical.
Dewatering ability is tested
In 10ml centrifuge tube, measure 8ml sample, put in centrifuge, rotate continuously with the speed of 3000r/min
15min, take out test tube, visual detection its whether be layered, testing result is as shown in the table:
| Embodiment | Testing result | Comparative example | Testing result |
| Embodiment 1 | Not stratified | Comparative example 1 | Layering |
| Embodiment 2 | Not stratified | Comparative example 2 | Layering |
| Embodiment 3 | Not stratified | Comparative example 3 | Layering |
As seen from the above table, defoamer prepared by the method for the present invention, dewatering ability is apparently higher than comparative example.
Claims (1)
1. an organic silicon defoamer, it is characterised in that according to weight portion meter, be made up of following raw material:
The silicon composition A of 5～30 parts, the polyether-modified polysiloxane B of 10～30 parts, the emulsifying agent C of 2～10 parts,
The coupling agent D of 0.01～0.1 part, the thickening agent E of 2～10 parts, the water of 30～60 parts；
Coupling agent D is selected from MTMS, MTES, amino trimethoxy silane or amino three ethoxy
Base silane；
The structural formula of described polyether-modified polysiloxane B is:
MDa(MeYSiO)bM
Wherein, M is chain link R3SiO1/2, D is chain link R2SiO2/2, R is identical or different, selected from hydrogen atom, the replacement of monovalence or non-take
The carbon number in generation is the alkyl of 1～20；Me is methyl；The structural formula of Y is :-(CH2)zO(EO)g(PO)hK, K are END CAPPED GROUP
Group, selected from hydrogen atom, methyl, ethyl, propyl group, butyl；Subscript a, b, z, g, h are the degree of polymerization, and a is the integer of 10～500, and b is 1
～the integer of 50, z is the integer of 2～6, and g is the integer of 1～36, and h is the integer of 0～20；
Described emulsifying agent C is NPE, OPEO, dodecyl phenol polyethenoxy ether and two nonyls
Base phenol polyethenoxy ether, lauric acid polyoxyethylene ether, oleic acid polyoxyethylene, Palmic acid polyoxyethylene ether, stearic acid polyoxy second
Alkene ether, fatty alcohol-polyoxyethylene ether, Sorbitan alcohol ether stearate polyoxyethylene ether or castor oil polyoxyethylene ether；
Described thickening agent E is selected from polyacrylamide, carbomer, HANSHENGJIAO, cellulose or polyacrylic acid.
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Cited By (4)
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|---|---|---|---|---|
| CN107737467A (en) * | 2017-10-23 | 2018-02-27 | 付海明 | Delayed coking antifoaming agent and its production and use |
| CN110960892A (en) * | 2019-11-29 | 2020-04-07 | 湖北新四海化工股份有限公司 | Efficient water-based paint defoaming agent and preparation method thereof |
| CN111040187A (en) * | 2019-11-28 | 2020-04-21 | 湖北新四海化工股份有限公司 | Organic silicon resin emulsion and preparation method thereof |
| CN112604325A (en) * | 2020-12-14 | 2021-04-06 | 浙江传化华洋化工有限公司 | Organic silicon modified unsaturated higher fatty alcohol ester defoaming agent and preparation method thereof |
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| CN111040187A (en) * | 2019-11-28 | 2020-04-21 | 湖北新四海化工股份有限公司 | Organic silicon resin emulsion and preparation method thereof |
| CN111040187B (en) * | 2019-11-28 | 2022-08-26 | 湖北新四海化工股份有限公司 | Organic silicon resin emulsion and preparation method thereof |
| CN110960892A (en) * | 2019-11-29 | 2020-04-07 | 湖北新四海化工股份有限公司 | Efficient water-based paint defoaming agent and preparation method thereof |
| CN112604325A (en) * | 2020-12-14 | 2021-04-06 | 浙江传化华洋化工有限公司 | Organic silicon modified unsaturated higher fatty alcohol ester defoaming agent and preparation method thereof |
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Application publication date: 20161214 |