CN109289255A - A kind of Sudo controlling compositions and preparation method thereof - Google Patents
A kind of Sudo controlling compositions and preparation method thereof Download PDFInfo
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- CN109289255A CN109289255A CN201811506022.XA CN201811506022A CN109289255A CN 109289255 A CN109289255 A CN 109289255A CN 201811506022 A CN201811506022 A CN 201811506022A CN 109289255 A CN109289255 A CN 109289255A
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- controlling compositions
- sudo controlling
- polysiloxane
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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
- B01D19/0409—Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
Abstract
The present invention relates to a kind of Sudo controlling compositions and preparation method thereof, Sudo controlling compositions are made by inert polysiloxane, containing vinyl polysiloxane, hydrogen containing siloxane, constitution controller, catalyst, silica, inertia organic siliconresin and water by mixing, addition.It is solved the problems, such as by the addition of the constitution controller and water of alkynol class sudden and violent poly- in implementation process, while also solving the problems, such as that viscosity becomes larger in Storage period.It can be used in the industries such as black liquid, textile printing and dyeing, sewage treatment, industry cleaning link with silicone foam control agents prepared by this method.
Description
Technical field
The present invention relates to a kind of Sudo controlling compositions based on polysiloxane, the composition is being rich in surface-active
There is excellent foam control performance in the industrial system of agent.The invention belongs to technical field of fine chemical preparations.
Background technique
Foam is phenomenon common in daily life and industrial processes, foam there are both advantageous and disadvantageous, such as people
It is frequently utilized that foam firefighting, manufactures food cake using the foam manufacture polyurethane of formation, using foam；And in many industrial bodies
Foam has production and living very big harm in system, because it influences yield and quality, environment and economic benefit.Eliminate foam
Method be generally divided into mechanical means and chemical method, so-called " mechanical means " is exactly using impacting with high pressure, increases temperature, makes
Foam is endangered with the elimination of the methods of negative pressure, but overall effect is bad；So-called " chemical method " be exactly with chemical agent, such as
Foam controls to eliminate foam, its basic principle is the variation by surface tension；Rather than by really chemically reacting
The concentration of foamer is reduced to eliminate foam.People, which are typically chosen with foam controller, eliminates, reduces or controls harm bubble
Foam.Currently, foam controller has been widely used for papermaking, coating, chemical industry, printing and dyeing, medicine, water process, food processing, petroleum
During exploitation etc..
It is well known that from the point of view of active material, relative to polyether-type, the foam control of fatty alcohol type, mineral oil origin
For agent, organic silicon type application range is most wide, and because having, dosage is small, defoaming capacity is strong, volatility is low, nontoxic, without side-effects
The advantages that and it is much favored by the market.The foam controller of organic silicon is mainly by polysiloxanes, hydrophobic particles, silicone resin and catalysis
The several fundamental components composition such as agent, US4639489 is initial foam controller, introduce by dimethyl silicone polymer and two
What silica was obtained by high temperature long-time working process, but such foam control composition structure is single, and suds suppressing properties are poor,
So far still by some industrial applications.Since the 1980s, the structure of polysiloxanes, the type of hydrophobic particles and use
Amount, the type of silicone resin, technical process etc. are all widely to be studied.US4338217A1 alkoxy polysiloxane with it is white
Silicone active object is made in carbon black particle mixed processing；US5824739 is directly with containing amino or carboxyl polysiloxanes and white carbon black
Mixed processing obtains silicon composition；US2008064806A1 has studied between the viscosity of silicon composition and foam inhibition effect
Otherness；CN201010213081.5 dimethyl silicone polymer, modified dimethyl polysiloxane mixing and white carbon black, silicon tree
Rouge prepares silicon cream；EP0163398A1 has studied height viscosity silicone and white carbon black is mixed with silicon cream.The system of these silicon cream
Standby is all around how the structure of polysiloxanes is studied.And introduced simultaneously in EP2794760 a kind of hydrophilic white carbon black and
A kind of hydrophobic silicic aerogels, and be reduced to the viscosity of composition by equipment such as colloid mills and heat preceding mixture measurement viscosity
50%, make defoaming composition finally in suitable viscosity in favor of emulsification, but the cross-linked structure that hydroxyl condensation is formed is more weak,
It is difficult to play good foam-inhibiting effect in the strong anion systems of foaming power.
By nearly research in 40 years, industry generally believes that the silicone foam control agents of excellent performance to be obtained have to do
At the polysiloxane composition of space structure.US5153258, which is introduced, introduces lightly crosslinked polysiloxanes and hard charcoal into system
It is black to mix to improve the antifoaming performance of composition.US8053480B2 equally describe a kind of big viscosity vinylsiloxane and
The hydrogen containing siloxane of small viscosity crosslinks reaction in the presence of hydrophobic silicic aerogels, until partial gelation, then it is high by applying
Shearing is on the mixture of this partial gelation until an appropriate viscosity range, the composition have relatively preferably in alkali system
Suds suppressing properties, but defoaming capacity is still short of, and the gelling that while preparing the composition generates is not easy to control.US3455839
A kind of vinyl polysiloxane and hydrogen containing siloxane are described with CA2074060 in transition-metal catalyst such as chloroplatinic acid item
The silicone antifoam compositions that the cross-linked structure of formation is reacted under part improve later period foam inhibition ability, but how to control and criticize
Otherness between secondary, is not yet received very good solution so far.
Preparing composition with vinyl polysiloxane and hydrogen containing siloxane for basic reactive material is foam control combination
One of object, the maximum problem of the composition of above-mentioned patent introduction is to be easy to occur to gather cruelly, so as to cause performance shakiness
Fixed or emulsion dispersion is highly difficult.
The present inventor's discovery when studying the reaction containing vinyl polysiloxane and hydrogen containing siloxane can pass through control
The addition of agent can control the degree of crosslinking, solves the problems, such as to gather cruelly, also just controls the difference of properties of product.
It can be used for black liquid, textile printing and dyeing, sewage treatment, work with Sudo controlling compositions prepared by this patent method
In the industries such as industry cleaning.
Summary of the invention
The present invention relates to a kind of Sudo controlling compositions and preparation method thereof.It is characterized in that, the foam composition
Object include inert polysiloxane, containing vinyl polysiloxane, hydrogen containing siloxane, constitution controller, catalyst, silica,
Inertia organic siliconresin and water:
A, inert polysiloxane
The inert polysiloxane general structure is as follows:
R a SiO(4-a)/2(I)
In formula (I),aValue be 1.9~2.2, the polysiloxanes including straight chain, branch and space structure；Substituent R is one
The alkyl that the substituted or non-substituted carbon atom number of valence is 1~30, value is identical or different, specifically includes:
Alkyl, such as methyl, ethyl, propyl, butyl, amyl, hexyl, octyl, decyl, 12 carbon alkyl, tetradecane base, 16
Carbon alkyl, octadecyl, icosane base, docosane base, tetracosa carbon alkyl, hexacosane base, 28 carbon
Alkyl, three decane bases；
Aromatic hydrocarbons, as phenyl,αMethylphenethyl；
Polyethers is mainly polymerized with allyl alcohol and ethylene oxide (EO) and propylene oxide (PO).
It is easy to get from raw material with from the point of view of cost, 80% substituent R is methyl in inert polysiloxane.
Dynamic viscosity of the inert polysiloxane at 25 DEG C is 100~10,000mPas.Inert polysiloxane
Dosage be silicon composition in gross mass 60 ~ 90%.
B, hydrogen containing siloxane
The general structure containing vinyl polysiloxane is as follows:
In formula (II), R1The alkyl or aryl with 1 ~ 8 carbon atom, as methyl, ethyl, propyl, amyl, hexyl, octyl,
Phenyl, styrene, preferably R1It is methyl；SubscriptbWithcIt is the degree of polymerization,bFor 0 or 1 ~ 5 integer, exist containing vinyl polysiloxane
Dynamic viscosity range at 25 DEG C is 200 ~ 80,000mPa.s, preferably 1000 ~ 40,000 mPa.s.It is described poly- containing vinyl
Siloxanes dosage is the 5 ~ 35% of Sudo controlling compositions gross mass.
C, hydrogen containing siloxane
The general structure of the hydrogen containing siloxane is as follows:
In formula (III), R2It is the alkyl or aryl of 1 ~ 8 carbon atom, such as methyl, ethyl, propyl, amyl, hexyl, octyl, benzene
Base, styrene, preferably R2It is methyl；R3It is hydrogen atom or methyl；SubscriptdIt is 0 or 1 ~ 10 integer, and exist in each molecule
At least two with the hydrogen atom of silicon bonding；SubscripteIndicate that integer, numerical value make the hydrogeneous polysiloxane at 25 DEG C
Dynamic viscosity range be 2 ~ 60mPa.s.The hydrogen containing siloxane dosage be Sudo controlling compositions gross mass 0.05 ~
8%。
D, constitution controller
The constitution controller is mainly the substance of alkynol class, selected from octyne alcohol, decine alcohol, 2- methyl -3- butyne-2-alcohol,
Methyl butynol, methylparafynol, 1- alkynyl cyclohexanol, 1,4- butynediols, 3,7,11- trimethyl dodecyne -3- alcohol, 4- penta
Alkynes -1- alcohol, 3,5- dimethyl -1- hexin -3- alcohol, 3- pentyne-1-alcohol, 3,5- dimethyl -1- hexin -3- alcohol, 3,6- diformazan
Base -4- octyne -3,6- glycol.
The dosage of the constitution controller is the 0.01 ~ 2% of Sudo controlling compositions gross mass.
E, catalyst
The catalyst is the precious metal catalyst for promoting hydrosilylation, is selected from platinum -ol complex compound, platinum-alkene
Complex compound, platinum -ol salt complex, platinum-ether complexes, platinum -one complex compound, chloroplatinic acid concentration are molten for 1% chloroplatinic acid isopropanol
Liquid, rhodium -ol complex compound, rhodium -ol salt complex, the isopropyl alcohol solution of chloroplatinic acid that preferred mass concentration is 1%.Catalyst amount is
3 ~ 30ppm of Sudo controlling compositions gross mass, preferably 5 ~ 15ppm(is in terms of platinum).
F, silica
Silica is divided into precipitated silica and fumed silica by manufacturing method, is divided into hydrophilic two by surface nature
Silica and hydrophobic silica.The present invention selects hydrophobic silica, including vapor phase method and the precipitation method, and specific surface area is 50 ~
500m2/ g, preferably 80 ~ 400m2/ g, the precipitating and gas-phase silica of different specific surface areas are used alone or be used in mixed way, and dosage is
Sudo controlling compositions gross mass is 3 ~ 10%.
G, inertia organic siliconresin
Inertia organic siliconresin is often referred to the silicone resin not chemically reacted substantially with other substances, usually by M chain link and Q chain
The molar ratio of the MQ resin of section composition, M chain link and Q chain link is (0.5 ~ 1.2): 1.0.The dosage of the inertia organic siliconresin is
The 1 ~ 8% of Sudo controlling compositions gross mass.
H, water
The water includes tap water, process water, pure water, and mode of appearance includes liquid water and solid ice.
The dosage of the water is the 0.1 ~ 2% of Sudo controlling compositions gross mass.
Sudo controlling compositions of the present invention the preparation method is as follows:
(1) inert polysiloxane, silica and inertia silicone resin are added in a reservoir, is heated to 40 ~ 120 DEG C, controls revolving speed
For 1000 ~ 3000rpm, so that solids are completely dispersed in inert polysiloxane, and made finally admittedly by milling apparatus
Body dispersion particle diameter is 5 μm hereinafter, to drop to room temperature spare, is denoted as dispersion I；
(2) it is added in another container and contains vinyl polysiloxane, hydrogen containing siloxane and constitution controller, increase temperature extremely
30 ~ 140 DEG C, stirring is denoted as mixture II so that mixture is transparent；
(3) dispersion I is added into mixture II, controls temperature at 50 ~ 100 DEG C, catalyst is added, then heat to 100 ~
150 DEG C, 0.5 ~ 4h is kept the temperature, thick liquid is obtained, is down to 90 DEG C or less addition water to temperature, is uniformly mixed, further dropped
To room temperature, Sudo controlling compositions of the invention are obtained.
Sudo controlling compositions prepared by the present invention can directly provide use according to the requirement of actual use, can also use
Solvent dilutes or lotion is made, or the foam control product of solid type is made.
The method for preparing the foam controller of oil-in-water emulsion form be it is known in those skilled in the art, one
As technical data on can inquire to obtain, this lotion generally by Sudo controlling compositions, emulsifier, water, thickener and
Preservative composition.
The nonionic surfactant includes that nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, lauric acid are poly-
Ethylene oxide ether, oleic acid polyoxyethylene, ethoxylated dodecyl alcohol, octanol polyoxyethylene ether, isooctanol polyethoxylate, isomery
Decyl alcohol polyoxyethylene ether, isomerous tridecanol polyoxyethylene ether, hexadecanol polyoxyethylene ether, polyoxyethylene octadecanol, dehydration mountain
Pears alcohol monolaurate, sorbitan monopalmitate, sorbitan monostearate, sorbitan monooleate,
Anhydrous sorbitol tristearate, sorbitan trioleate, polyoxyethylene 20 sorbitan monolaurate, polyoxyethylene
Sorbitan monopalmitate, polyoxyethylene 20 sorbitan monostearate, polyoxyethylene 20 sorbitan monooleate,
Polyoxyethylene 20 sorbitan tristearate, polyoxyethylene 20 sorbitan trioleate, in castor oil polyoxyethylene ether
One or more mixtures, preferably a variety of mixtures.
Thickener is selected from polyacrylamide, polyvinyl alcohol, carbomer, xanthan gum, polyacrylate, cellulose ethers, excellent
The thickener of xanthan gum and polyacrylate is selected, dosage is adjusted according to the requirement of emulsion viscosity.
Specific embodiment
Embodiment 1
It is the dimethyl silicone polymer of 1000mPas trimethyl silicane sealing end, 3 parts of specific surfaces that 85.13 parts of viscosity are added in a reservoir
Product is 200m2(molar ratio of M chain link and Q chain link is for the hydrophobic fumed silica R974 of/g and 1.3 parts of inertia organic siliconresins
0.7:1.0 is heated to 45 DEG C, and control revolving speed is 3000rpm, so that solids are completely dispersed in inert polysiloxane, and
Make final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, is denoted as dispersion I；
10 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=0, viscosity 20,000mPa
S), 0.06 part of hydrogen containing siloxane (R2For methyl, R3For methyl,d=0, viscosity 25mPas) and 0.01 part of Isosorbide-5-Nitrae-butine
Glycol, maintains the temperature at 35 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 50 DEG C, chloroplatinic acid/aqueous isopropanol of 10ppm is added (with platinum
Meter), 100 DEG C are then heated to, 4h is kept the temperature, obtains thick liquid, be down to 88 DEG C of additions, 0.5 part of water to temperature, is stirred
It is even, it is further reduced to room temperature, obtains Sudo controlling compositions FC-1 of the invention, dynamic viscosity when testing 25 DEG C is 93,
000mPa·s。
Embodiment 2
The polydimethylsiloxanes that the cetyl that 60.8 parts of viscosity are 100mPas trimethyl silicane sealing end is modified are added in a reservoir
Alkane, 5 parts of specific surface areas are 380m2Hydrophobic fumed silica 830 and 3 part powdery inertia organic siliconresin (M chain link and the Q of/g
The molar ratio of chain link is 0.5:1.0, is heated to 120 DEG C, control revolving speed is 1000rpm, so that solids are in the poly- silicon oxygen of inertia
It is completely dispersed in alkane, and makes final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, be denoted as point
Granular media I；
30 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=1, viscosity 40,000mPa
S), 0.2 part of hydrogen containing siloxane (R2For methyl, R3For hydrogen atom,d=10, viscosity 58mPas) and 0.5 part of methyl pentyne
Alcohol, maintains the temperature at 135 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 100 DEG C, chloroplatinic acid/aqueous isopropanol of 11ppm is added (with platinum
Meter), 150 DEG C are then heated to, 0.5h is kept the temperature, obtains thick liquid, is down to 80 DEG C of additions, 0.5 part of trash ice to temperature, stirring is mixed
It closes uniformly, is further reduced to room temperature, obtains Sudo controlling compositions FC-2 of the invention, dynamic viscosity when testing 25 DEG C is
157,000mPa·s。
Embodiment 3
It is 2000mPas trimethyl silicane sealing end that 76.2 parts of viscosity are added in a reservoirαThe modified poly- diformazan of methyl styrene
Radical siloxane, 5 parts of specific surface areas are 80m2The precipitating hydrophobic silica D10 of/g and 7 parts of inertia organic siliconresins (M chain link and Q
The molar ratio of chain link is 1.2:1, is heated to 100 DEG C, control revolving speed is 2500rpm, so that solids are in inert polysiloxane
In be completely dispersed, and make final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, be denoted as dispersion
Body I；
5 parts of (R containing vinyl polysiloxane are added in another container1ForαMethyl styrene,b=5, viscosity 1,
000mPas), 8 parts of hydrogen containing siloxane (R2ForαMethyl styrene, R3For hydrogen atom,d=1, viscosity 20mPas) and 2
Part 1- alkynyl cyclohexanol maintains the temperature at 115 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 80 DEG C, chloroplatinic acid/aqueous isopropanol of 9ppm is added (with platinum
Meter), 120 DEG C are then heated to, 2h is kept the temperature, obtains thick liquid, be down to 75 DEG C of 0.9 part of trash ices of addition and 0.9 part of water to temperature,
It is uniformly mixed, is further reduced to room temperature, obtain Sudo controlling compositions FC-3 of the invention, power when testing 25 DEG C glues
Degree is 33,000mPas.
Embodiment 4
The poly dimethyl silicon that the cetyl that 74.1 parts of viscosity are 1400mPas trimethyl silicane sealing end is modified is added in a reservoir
Oxygen alkane, 6 parts of specific surface areas are 80m2The precipitating hydrophobic silica D10 of/g, 3 parts of specific surface areas are 380m2The hydrophobic gas phase two of/g
(molar ratio of M chain link and Q chain link is 0.66:1 to silica 830 and 2 part inertia organic siliconresin, is heated to 80 DEG C, controls revolving speed
For 1500rpm, so that solids are completely dispersed in inert polysiloxane, and by milling apparatus final solid is dispersed
Partial size is 5 μm hereinafter, to drop to room temperature spare, is denoted as dispersion I；
4 parts of (R containing vinyl polysiloxane are added in another container1For cetyl,b=3, viscosity 30,000mPa
S), 8 parts of hydrogen containing siloxane (R2For cetyl, R3For methyl,d=1, viscosity 38mPas) and 1.5 parts of 3,5- diformazans
Base -1- hexin -3- alcohol, maintains the temperature at 105 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 100 DEG C, chloroplatinic acid/aqueous isopropanol of 8ppm is added (with platinum
Meter), 130 DEG C are then heated to, 1.5h is kept the temperature, obtains thick liquid, be down to 85 DEG C of additions, 1.4 parts of water to temperature, be stirred
Uniformly, it is further reduced to room temperature, obtains Sudo controlling compositions FC-4 of the invention, dynamic viscosity when testing 25 DEG C is 47,
000mPa·s。
Embodiment 5
The polyether-modified dimethyl silicone polymer that 65.2 parts of viscosity are 1400mPas trimethyl silicane sealing end is added in a reservoir
(CH2CH2CH2O(EO)5(PO)18H), 5 parts of specific surface areas are 150m2The hydrophobic fumed silica R972 of/g and 3 parts of inertia have
(molar ratio of M chain link and Q chain link is 0.75:1 to machine silicone resin, is heated to 100 DEG C, control revolving speed is 2000rpm, so that solid
Particle is completely dispersed in inert polysiloxane, and makes final solid dispersion particle diameter be 5 μm hereinafter, dropping to by milling apparatus
Room temperature is spare, is denoted as dispersion I；
25 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=4, viscosity 23,000mPas),
0.8 part of hydrogen containing siloxane (R2For methyl, R3For methyl,d=1, viscosity 48mPas) and 3,5- dimethyl -1- hexin -
3- alcohol, maintains the temperature at 115 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 85 DEG C, chloroplatinic acid/aqueous isopropanol of 5ppm is added (with platinum
Meter), 150 DEG C are then heated to, 3.5h is kept the temperature, obtains thick liquid, be down to 85 DEG C of additions, 1.0 parts of water to temperature, be stirred
Uniformly, it is further reduced to room temperature, obtains Sudo controlling compositions FC-5 of the invention, dynamic viscosity when testing 25 DEG C is 130,
000mPa·s。
Embodiment 6
Be added in a reservoir 71.7 parts of viscosity be the dimethyl silicone polymer of 10,000mPas trimethyl silicane sealing end, 3 parts compare table
Area is 90m2(molar ratio of M chain link and Q chain link is for the hydrophobic precipitating aerosil D10 of/g and 6 parts of inertia organic siliconresins
0.7:1.0 is heated to 45 DEG C, and control revolving speed is 3000rpm, so that solids are completely dispersed in inert polysiloxane, and
Make final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, is denoted as dispersion I；
18 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=0, viscosity 20,000mPa
S), 0.5 part of hydrogen containing siloxane (R2For methyl, R3For methyl,d=0, viscosity 25mPas) and Isosorbide-5-Nitrae-butynediols, it protects
Temperature is held at 35 DEG C, stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 50 DEG C, chloroplatinic acid/aqueous isopropanol of 10ppm is added (with platinum
Meter), 100 DEG C are then heated to, 4h is kept the temperature, obtains thick liquid, be down to 88 DEG C of additions, 0.8 part of water to temperature, is stirred
It is even, it is further reduced to room temperature, obtains Sudo controlling compositions FC-6 of the invention, dynamic viscosity when testing 25 DEG C is 115,
000mPa·s。
Embodiment 7
It is the dimethyl silicone polymer of 5,000mPas trimethyl silicane sealing end, 4 parts of specific surfaces that 72.4 parts of viscosity are added in a reservoir
Product is 200m2(molar ratio of M chain link and Q chain link is for the hydrophobic gas phase aerosil R202 of/g and 3 parts of inertia organic siliconresins
0.60:1.0 is heated to 85 DEG C, and control revolving speed is 2300rpm, so that solids are completely dispersed in inert polysiloxane, and
Make final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, is denoted as dispersion I；
15 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=2, viscosity 15,000mPa
S), 2 parts of hydrogen containing siloxane (R2For methyl, R3For hydrogen atom,d=5, viscosity 58mPas) and 1.6 parts of 3,6- dimethyl-
4- octyne -3,6- glycol, maintains the temperature at 105 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 75 DEG C, chloroplatinic acid/aqueous isopropanol of 14ppm is added (with platinum
Meter), 120 DEG C are then heated to, 3h is kept the temperature, obtains thick liquid, be down to 83 DEG C of additions, 2 parts of water to temperature, be uniformly mixed,
It is further reduced to room temperature, obtains Sudo controlling compositions FC-7 of the invention, dynamic viscosity when testing 25 DEG C is 146,
000mPa·s。
Embodiment 8 ~ 10
1kg, 10kg, 100kg amplification are carried out according to the proportion of embodiment 7, obtains FC-8, FC-9, FC-10, when testing 25 DEG C
Dynamic viscosity is respectively 128,000mPas, 154,000mPas, 145,000mPas.
Comparative example 1
It is the dimethyl silicone polymer of 5,000mPas trimethyl silicane sealing end, 4 parts of specific surfaces that 74.4 parts of viscosity are added in a reservoir
Product is 200m2(molar ratio of M chain link and Q chain link is for the hydrophobic gas phase aerosil R202 of/g and 3 parts of inertia organic siliconresins
0.60:1.0 is heated to 85 DEG C, and control revolving speed is 2300rpm, so that solids are completely dispersed in inert polysiloxane, and
Make final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, is denoted as dispersion I；
15 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=2, viscosity 15,000mPa
S), 2 parts of hydrogen containing siloxane (R2For methyl, R3For hydrogen atom,d=5, viscosity 58mPas) and 1.6 parts of 3,6- dimethyl-
4- octyne -3,6- glycol, maintains the temperature at 105 DEG C, and stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 75 DEG C, chloroplatinic acid/aqueous isopropanol of 14ppm is added (with platinum
Meter), 120 DEG C are then heated to, 3h is kept the temperature, obtains thick liquid, be down to room temperature, obtain Sudo controlling compositions CFC-7A, is surveyed
Dynamic viscosity when trying 25 DEG C is 140,000mPas.
Comparative example 2:
It is the dimethyl silicone polymer of 5,000mPas trimethyl silicane sealing end, 4 parts of specific surface areas that 74 parts of viscosity are added in a reservoir
For 200m2(molar ratio of M chain link and Q chain link is for the hydrophobic gas phase aerosil R202 of/g and 3 parts of inertia organic siliconresins
0.60:1.0 is heated to 85 DEG C, and control revolving speed is 2300rpm, so that solids are completely dispersed in inert polysiloxane, and
Make final solid dispersion particle diameter be 5 μm by milling apparatus hereinafter, to drop to room temperature spare, is denoted as dispersion I；
15 parts of (R containing vinyl polysiloxane are added in another container1For methyl,b=2, viscosity 15,000mPa
S), 2 parts of hydrogen containing siloxane (R2For methyl, R3For hydrogen atom,d=5, viscosity 58mPas), 105 DEG C are maintained the temperature at,
Stirring is denoted as mixture II so that mixture is transparent；
Dispersion I is added into mixture II, controls temperature at 75 DEG C, chloroplatinic acid/aqueous isopropanol of 14ppm is added (with platinum
Meter), 120 DEG C are then heated to, 3h is kept the temperature, obtains thick liquid, be down to 83 DEG C of additions, 2 parts of water to temperature, be uniformly mixed,
It is further reduced to room temperature, obtains Sudo controlling compositions CFC-7B, dynamic viscosity when testing 25 DEG C is 230,000mPas.
Comparative example 3:
According to the method preparation of example 2 in CN101454061A, Sudo controlling compositions CFC-7B is obtained, power when testing 25 DEG C
Viscosity is 78,000mPas.
The test of foam control performance:
The preparation of test sample: using hexamethylene as dilution medium, Sudo controlling compositions are diluted
Tested media: 1%NP-10 aqueous solution
Test method: it is tested using shaking flask method
Test method: have the above-mentioned frothing media 50mL of additional amount in plug graduated cylinder toward 100mL, then add the test specimens of 0.010g
Product are stood after amplitude shake 50 times of 30~40cm in vertical direction with the frequency of 100~120 times/min, and record foam disappears
It is foam time, then 50 record foam times of shake to there is the liquid level time, when until total shaking flask number reaching 400 times
Between it is shorter, then the defoaming composition foam inhibition effect that disappears is better.
The foam control performance test result of silicon composition is as shown in table 1:
By the data of table 2 it can be seen that
(1) ability of the control foam of embodiment 1 ~ 10 is relatively good；
(2) embodiment 8 ~ 10 is the amplification test carried out on the basis of embodiment 7, also shows preferable effect；
(3) water is not added in comparative example CFC-7A, has not significant impact to the ability of foam control, but the control of CFC-7B is steeped
The ability ratio FC-7 and CFC-7A of foam is poor, this is because being easy to produce sudden and violent poly- phenomenon in the case where without controlling agent, causing to glue
Degree is very big, is not easy to disperse in bubble medium.
Comparison CFC-7C and remaining embodiment result can be seen that by the addition of micro water and constitution controller with
And the control of technique, the more excellent performance of composition than existing patent can be obtained.
Stability test:
Viscosity change after comparing initial viscosity and putting under room temperature one month, the results are shown in Table 2:
By the data of table 2 it can be seen that
(1) viscosity change of the composition of embodiment 1 ~ 10 after putting one month does not influence subsequent cream within 10%
Change application；
(2) the composition of constitution controller can not generate sudden and violent gather in implementation process；Plus in the implementation process of water do not have
Have and gather cruelly, but viscosity change is very big during putting, and can seriously affect the use in later period；
(3) in short, can solve hydrogen containing siloxane and the poly- silicon oxygen of vinyl by the addition of the constitution controller and water of alkynol class
The sudden and violent poly- problem of alkane, also can be effectively controlled the growth of later period viscosity.
Claims (9)
1. a kind of Sudo controlling compositions, which is characterized in that the foam compositions include inert polysiloxane, containing vinyl
Polysiloxanes, hydrogen containing siloxane, constitution controller, catalyst, silica, inertia organic siliconresin and water:
A, inert polysiloxane, dynamic viscosity of the inert polysiloxane at 25 DEG C are 100~10,000mPas, are used
Amount is 60 ~ 90% of gross mass in silicon composition；
B, contain vinyl polysiloxane, the dosage containing vinyl polysiloxane is the 5 ~ 35% of Sudo controlling compositions gross mass；
C, hydrogen containing siloxane, the hydrogen containing siloxane dosage are the 0.05 ~ 8% of Sudo controlling compositions gross mass；
D, constitution controller, the constitution controller are selected from octyne alcohol, decine alcohol, 2- methyl -3- butyne-2-alcohol, methyl fourth
Alkynol, methylparafynol, 1- alkynyl cyclohexanol, 1,4- butynediols, 3,7,11- trimethyl dodecyne -3- alcohol, 4- pentyne -1-
Alcohol, 3,5- dimethyl -1- hexin -3- alcohol, 3- pentyne-1-alcohol, 3,5- dimethyl -1- hexin -3- alcohol, 3,6- dimethyl -4- are pungent
Alkynes -3,6- glycol；Dosage is the 0.01 ~ 2% of Sudo controlling compositions gross mass；
E, catalyst, the catalyst are selected from platinum -ol complex compound, platinum-alkene complex, platinum -ol salt complex, platinum-ether complexing
Object, platinum -one complex compound, the isopropyl alcohol solution of chloroplatinic acid that chloroplatinic acid concentration is 1%, rhodium -ol complex compound, rhodium -ol salt complex, it is excellent
Selecting chloroplatinic acid concentration is 1% isopropyl alcohol solution of chloroplatinic acid；Catalyst amount is 3 ~ 30ppm of Sudo controlling compositions gross mass；
F, silica, the silica include vapor phase method and the precipitation method, and specific surface area is 50 ~ 500m2/ g, not year-on-year table
The precipitating and gas-phase silica of area are used alone or be used in mixed way, and dosage is that Sudo controlling compositions gross mass is 3 ~ 10%；
G, inertia organic siliconresin, the MQ resin that the inertia organic siliconresin is made of M chain link and Q chain link, M chain link and Q
The molar ratio of chain link is (0.5 ~ 1.2): 1.0；Dosage is the 1 ~ 8% of Sudo controlling compositions gross mass；
H, water, the water include tap water, process water, pure water, and mode of appearance includes liquid water and solid ice；Dosage is
The 0.1 ~ 2% of Sudo controlling compositions gross mass；
The Sudo controlling compositions the preparation method is as follows:
(1) inert polysiloxane, silica and inertia silicone resin are added in a reservoir, is heated to 40 ~ 120 DEG C, controls revolving speed
For 1000 ~ 3000rpm, so that solids are completely dispersed in inert polysiloxane, and made finally admittedly by milling apparatus
Body dispersion particle diameter is 5 μm hereinafter, to drop to room temperature spare, is denoted as dispersion I；
(2) it is added in another container and contains vinyl polysiloxane, hydrogen containing siloxane and constitution controller, increase temperature extremely
30 ~ 140 DEG C, stirring is denoted as mixture II so that mixture is transparent；
(3) dispersion I is added into mixture II, controls temperature at 50 ~ 100 DEG C, catalyst is added, then heat to 100 ~
150 DEG C, 0.5 ~ 4h is kept the temperature, thick liquid is obtained, is down to 90 DEG C or less addition water to temperature, is uniformly mixed, further dropped
To room temperature, Sudo controlling compositions of the invention are obtained.
2. a kind of Sudo controlling compositions according to claim 1, which is characterized in that the inert polysiloxane structure
General formula is as follows:
R a SiO(4-a)/2(I)
In formula (I),aValue be 1.9~2.2, the polysiloxanes including straight chain, branch and space structure；Substituent R is one
The alkyl that the substituted or non-substituted carbon atom number of valence is 1~30, value is identical or different, including alkyl, aromatic hydrocarbons and by allyl
The allyl alcohol polyether that alcohol and ethylene oxide (EO), propylene oxide (PO) are polymerized.
3. a kind of Sudo controlling compositions according to claim 2, which is characterized in that be easy to get the angle with cost from raw material
Consider, 80% substituent R is methyl in inert polysiloxane structural formula.
4. a kind of Sudo controlling compositions according to claim 1, which is characterized in that described contains vinyl polysiloxane
General structure it is as follows:
In formula (II), R1It is the alkyl or aryl with 1 ~ 8 carbon atom, preferably R1It is methyl；SubscriptbWithcIt is the degree of polymerization,bFor
0 or 1 ~ 5 integer, the dynamic viscosity range containing vinyl polysiloxane at 25 DEG C are 200 ~ 80,000mPas.
5. a kind of Sudo controlling compositions according to claim 4, which is characterized in that described contains vinyl polysiloxane
The dynamic viscosity at 25 DEG C range preferably from 1000 ~ 40,000 mPas.
6. a kind of Sudo controlling compositions according to claim 1, which is characterized in that the knot of the hydrogen containing siloxane
Structure general formula is as follows:
In formula (III), R2It is the alkyl or aryl of 1 ~ 8 carbon atom, preferably R2It is methyl；R3It is hydrogen atom or methyl；SubscriptdIt is
0 or 1 ~ 10 integer, and there are at least two and the hydrogen atom of silicon bonding in each molecule；SubscripteIndicate that integer, numerical value make
Obtaining dynamic viscosity range of the hydrogeneous polysiloxane at 25 DEG C is 2 ~ 60mPas.
7. a kind of Sudo controlling compositions according to claim 1, which is characterized in that the high quality concentration of catalyst is
1% isopropyl alcohol solution of chloroplatinic acid.
8. a kind of Sudo controlling compositions according to claim 1, which is characterized in that the dosage of the catalyst is foam
5 ~ 15ppm(of control composition gross mass is in terms of platinum).
9. a kind of Sudo controlling compositions according to claim 1, which is characterized in that the specific surface of the silica
Product is preferably 80 ~ 400m2/g。
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| CN109758794A (en) * | 2019-03-20 | 2019-05-17 | 南京瑞思化学技术有限公司 | A kind of preparation method of silicon composition |
| CN111056765A (en) * | 2019-12-06 | 2020-04-24 | 江苏四新科技应用研究所股份有限公司 | Defoaming agent applied to thin-layer self-leveling mortar and preparation method thereof |
| CN115340769A (en) * | 2022-10-03 | 2022-11-15 | 南京瑞思化学技术有限公司 | Preparation method of organic silicon composition |
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| CN111056765A (en) * | 2019-12-06 | 2020-04-24 | 江苏四新科技应用研究所股份有限公司 | Defoaming agent applied to thin-layer self-leveling mortar and preparation method thereof |
| CN111056765B (en) * | 2019-12-06 | 2021-11-19 | 江苏四新科技应用研究所股份有限公司 | Defoaming agent applied to thin-layer self-leveling mortar and preparation method thereof |
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| CN115340769B (en) * | 2022-10-03 | 2023-10-27 | 南京瑞思化学技术有限公司 | Preparation method of organic silicon composition |
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