CN110256692A - A method of improving stability of organic silicone emulsion - Google Patents
A method of improving stability of organic silicone emulsion Download PDFInfo
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- CN110256692A CN110256692A CN201910541832.7A CN201910541832A CN110256692A CN 110256692 A CN110256692 A CN 110256692A CN 201910541832 A CN201910541832 A CN 201910541832A CN 110256692 A CN110256692 A CN 110256692A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/10—Block- or graft-copolymers containing polysiloxane sequences
- C08J2483/12—Block- or graft-copolymers containing polysiloxane sequences containing polyether sequences
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Abstract
The present invention provides a kind of methods for improving stability of organic silicone emulsion, comprising: active material, higher aliphatic polyethers, emulsifier and Siloxane-Oxyalkylene Copolymers;Method includes: R1: active material, higher aliphatic polyethers, emulsifier, silicon polyethers are sufficiently mixed 10-50min, preferably 15min-30min under stiring;R2: it completes that the temperature of above-mentioned system is increased to 55 DEG C -85 DEG C after above-mentioned R1, then system temperature is kept, it is slowly added into water, improving mixing speed makes it become O/W type emulsion inverse from w/o type lotion, continue to add water to required mass concentration, generally 40%-70%, preferably 50%-65%;R3: thick lotion is further emulsified by colloid mill in above-mentioned R2, is finally diluted to required emulsion concentration with viscous water.Higher aliphatic polyethers is added when emulsifying organosilicon mixture into mixture by the present invention, can greatly improve the emulsifying power of emulsifier, obtain more stable organic silicon emulsion, greatly promote the function of active material in this way.
Description
Technical field
The present invention relates to the preparations of fine chemicals additive, belong to technical field of fine chemical preparations technical field, tool
Body is related to a kind of method for improving stability of organic silicone emulsion.
Background technique
Organic silicon emulsion is important one of organosilicon product, due to its special performance and feature, industrially obtains
It is widely applied, is widely used in papermaking, weaving, slurry, coating, building, leather, medicine, cosmetics etc., and application neck
Domain is constantly open, and application potential is very big.In above-mentioned application field, organosilicon uses the most economic, side in the form of aqueous emulsion
Just, safety, while meeting the requirement of environmental protection.Organic silicon emulsion used in industrial process is mainly oil-in-water type (O/W), O/
The preparation of W type organic silicon emulsion there are mainly two types of preparation method, the first is formed by the method for polymerization, will be organic
Silicon monomer the catalyst and initiator and surfactant the effects of under be polymerized, such as fabric water repellent agent;It is for second
It is prepared by mechanical method, the various components, including oil phase component, emulsifier, water, stabilizer etc. of lotion will be prepared, led to
It crosses the modes such as heating stirring, mechanical shearing, colloid mill, homogenizer to disperse to be made, such as defoaming agent, release agent.According to organic
The difference of silicon emulsion usage, the polysiloxanes for selecting different viscosities, modified polyorganosiloxane are as active material, these poly- silicon
Oxygen alkane has plenty of linear structure, has plenty of space three-valued structures, disperses water for active material with a kind of emulsion preparation method
In be the very difficult thing of part, patent CN1807512 and CN101298027 highly viscous will be mixed by the way that some auxiliary substances are added
Object is closed to be dispersed in water.In fact, the function of organic silicon emulsion is fully ensured that, it is necessary to by the function of lotion property relevant with remaining
Matter is closely connected together, for example, organic silicon defoamer lotion must also consider product while guaranteeing antifoam performance
Dilution stability, shear resistant, storage stability and resistance to temperature stability etc.;, whereas if by bad organic of stability
Silicon emulsion defoaming agent is applied to if eliminating unwanted bubbles in the dyeing such as cotton, chemical fibre in textile industry, is just readily formed " silicon
Spot " seriously affects the efficiency of dyeing and the quality of final products, causes heavy losses economically.Therefore, organic silicon emulsion
Stabilization be comparable important.Organic silicon emulsion includes active material, emulsifier, stabilizer, fungicide and water etc..Emulsifier master
If being used to dispersed actives, a large amount of experiment experience shows that emulsifier is excessive, influences the main function of organic silicon emulsion
Energy;Emulsifier is very few, then organic silicon emulsion is very unstable, is likely to result in loss.Therefore, many organic silicon emulsion researchers are
Pay close attention to " when guaranteeing the performance security of organic silicon emulsion, how reducing the ratio between emulsifier and active material? " to fill
The function of active material is waved in distribution, reduces chemical oxygen consumption (COC) (COD) and biological oxygen consumption (BOD), realizes low-carbon economy and environmental protection
It is economical.
Currently, being dispersed using silicon polyethers, anhydrous sorbitol polyether derivative, alkyl phenol polyether derivative etc. as emulsifier
Organosilicon mixture is main method, but the emulsifying power of these emulsifiers needs to be further increased.
Summary of the invention
In view of the foregoing drawbacks, it is an object of the present invention to provide a kind of method for improving stability of organic silicone emulsion, solves
State background technique there are the problem of, meet application request.
The present invention is achieved by the following technical solutions:
The object of the present invention is to provide a kind of methods for improving stability of emulsion, and the lotion mainly includes following several groups
Point:
1, active material:
The active material includes polysiloxane, hydrophobic particles and catalyst;
(1) general structure of the polysiloxane described in is as follows: RaSiO(4-a)/2
Wherein R be substituted or non-substituted monovalent hydrocarbon, carbon atom number 1-20, these groups include alkyl such as methyl,
Ethyl, propyl, isopropyl, butyl, isobutyl group;Aryl (phenyl, tolyl, benzyl) and alkylene (including vinyl, propylene
Base), hydrogen moiety in these groups or all replaced halogen atom, cyano, for example (,) chloromethyl, 3,3,3- trifluoropropyls
The value of base, a is 1.9-2.2, and there are many polysiloxane for meeting conditions above, refer to trimethyl silicane oxygen in the present invention
The dimethyl silicone polymer of base sealing end, viscosity 10-100,000mPas, preferably 100-10,000mPas, dosage are
The 80-99% of defoaming activity object, preferably 90-95%;
(2) hydrophobic particles described in mainly have the oxide of the silicon of surface hydrophobicity of the partial size less than 25 μm, magnesium, zinc, aluminium, such as
Silica, magnesia, zinc oxide, aluminum oxide, what the present invention selected is hydrophobic silica, and specific surface area is at least
50m2/ g, preferably 150-250m2/ g, dosage account for the 0-18% of active material, preferably 3-8%;
(3) catalyst described in is broken by polysiloxane chain, so that between polysiloxanes and silica further
React, further increase the hydrophobicity of hydrophobic silica, common catalyst include LiOH, CsOH, NaOH, KOH,
Me4NOH, H2SO4, H3PO4, the preferred NaOH of the present invention, the dosage of catalyst are the 0-3%, preferably 1-2% of active material;
The preparation process of the active material is as follows: first polysiloxanes and silica is uniformly mixed at room temperature, with
Holding comes into full contact with;Then it is warming up to reaction temperature, reaction temperature is 50-300 DEG C, preferably 100-200 DEG C, and catalyst is added
2-8h, preferably 4-6h are reacted, end of reaction is cooled to room temperature up to active material.
2, higher aliphatic polyethers
Higher aliphatic polyethers used in the present invention is the catalysis using higher aliphatic as initiator, in catalyst and epoxy
The polymer that polymerization reaction obtains occurs for ethane (EO), propylene oxide (PO), and general formula is as follows: R1O(EO)m(PO)nH;
R1For the initiator of higher aliphatic polyethers, R1For alkyl, carbon atom number is the alkane of the linear chain or branched chain of 12-24
Base, including dodecyl, myristyl, cetyl, octadecyl and docosyl.The preferred carbon atom number of R1 is 16-20
Straight chained alkyl, m, n are the degree of polymerization, the integer that the integer that m is 5-50 preferred 10-25, n are 10-80, preferably 20-50 in formula;
Usually according to the mass fraction, the active material is 100%, then higher aliphatic polyethers is selected as 5~30%,
It is preferred that 5~20%.
3, emulsifier
Emulsifier in the present invention comprising nonionic surfactant, anionic surfactant, cationic surface are living
Property agent and amphoteric surfactant;
The example of nonionic surfactant is nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, lauric acid polyoxy
Vinethene, oleic acid polyoxyethylene, sorbitan monostearate, sorbitan monooleate, anhydrous sorbitol three are hard
Resin acid ester, sorbitan trioleate, anhydrous sorbitol monostearate polyoxyethylene ether-ester, anhydrous sorbitol list oleic acid polyoxy
Ethylene ether-ether, three stearic acid polyoxyethylene ether ester of anhydrous sorbitol, castor oil polyoxyethylene ether, alkyl phenol polyoxyethylene ether and
It is such.
The example of anionic surfactant is nonylphenol polyoxyethylene ether sulfate, octyl phenol polyoxyethylene ether sulfuric acid
The surfactant of salt, alkylphosphonic and the like.
The example of cationic surfactant is alkyl benzyl ammonium salt, lauric acid imidazoline, oleoyl imidazoline, hexadecane
The surfactant of the salt of base amine and the like.
The example of amphoteric surfactant is the amophoteric surface active of the own lactones type of alkyltrimethylammonium, phosphate type
Agent.
Preferred nonionic surfactants, the nonionic surfactant used are one or more mixtures, preferably
A variety of mixtures.
Usually based on mass parts score, the active material is 100%, then emulsifier is selected as 0~30%, preferably 5
~15%.
4, Siloxane-Oxyalkylene Copolymers
Siloxane-Oxyalkylene Copolymers are commonly called as silicon polyethers, be by hydrogen containing siloxane and unsaturated polyether catalyst work
It is prepared with lower generation addition reaction;Dynamic viscosity of the silicon polyethers at 25 DEG C be 10~30,000mPas, it is excellent
It is selected as 60~5, the 000mPas at 25 DEG C, the structural formula of silicon polyethers is as follows: MDx(CH3GSiO)yM;
Wherein, alphabetical M represents the chain link R in organic siliconresin2 3SiOl/2, D is chain link R2 2SiO2/2, the R of two structural formulas2It takes
It is identical to be worth range;G is polyether group, is indicated with general structure the following :-(CH2)z(EO)g(PO)hR3
R in formula3For-H or-CH3Or-COCH3;Above-mentioned each structural formula subscript x, y, z, g, h are the degree of polymerization, x 10-
500 integer;Y is the integer of 1-50;Z is the integer of 2-6;G is 1-36 integer;H is the integer of 0-20.
Usually according to the mass fraction, the active material is 100%, then silicon polyethers be selected as 5~30%, preferably 5~
20%.
According to the requirement to emulsion viscosity, thickener can be added, thickener include polyacrylamide, carbomer, xanthan gum,
The dosage of polyacrylate, cellulose ethers, thickener is adjusted according to the viscosity of lotion, is needed when long term storage to be added and be killed
Microbial inoculum and preservative, such as sodium hypochlorite, potassium sorbate, s-triazine, Kathon.
The method of preparation lotion has " agent-in-water method ", " agent-in-oil method ", " nascent soap method " etc., and the present inventor selects
" agent-in-oil method " prepares the water dispersion lotion of high-viscosity organosilicon composition, and the specific method is as follows:
At room temperature, active material, higher aliphatic polyethers, emulsifier, silicon polyethers are sufficiently mixed 10 under stiring~
50min, preferably 15min~30min;The temperature of above-mentioned system is increased to 55 DEG C~85 DEG C after the completion;Then, system temperature is kept
Degree is slowly added into water, and improving mixing speed makes it become O/W type emulsion inverse from w/o type lotion, continues required for adding water to
Mass concentration, generally 40%~70%, preferably 50%~65%;Thick lotion is further emulsified by colloid mill;Finally
Required emulsion concentration is diluted to viscous water.
Beneficial effects of the present invention:
The performance of high-viscosity organosilicon composition lotion prepared by the present invention is mainly assessed from the following aspects:
(1) stability of water diluent: being added in 99% water according to 1% organic silicon emulsion, after being uniformly dispersed, sees
Examine the liquid level situation of water diluent.
(2) it the high-temperature stability of water diluent: is added in 99% water according to 1% organic silicon emulsion, is seen after heating
Examine the liquid level situation of water diluent.
(3) under room temperature, lotion stoste the anti-shear performance of lotion: is placed on to the frequency of 100 times/min on horizontal oscillator tube
Rate vibrates 30min and compares the liquid level situation of water diluent according to the method for above-mentioned (1).
(4) lotion: being placed in 48h in 40 DEG C of baking oven by the high temperature resistance of lotion, according to the side of above-mentioned (1) and (2)
The liquid level situation of method observation water diluent.
In summary: higher aliphatic polyethers is added when emulsifying organosilicon mixture into mixture by the present invention, can be big
The big emulsifying power for improving emulsifier, obtains more stable organic silicon emulsion, greatly promotes the function of active material in this way.
Specific embodiment
Embodiment 1:
The preparation of active matter
The white carbon black that the dimethyl silicone polymer and 4% trade mark that viscosity by 94% is 1000mPa.s are A-200 is in room temperature
It is lower to be uniformly mixed, and 2%NaOH is added, 5h is then kept at 150 DEG C, and negative pressure state is remained in system, it is low to remove
Molecule.It is cooled to room temperature, obtains active matter A.
Embodiment 2:
The preparation of active matter
The white carbon black that the dimethyl silicone polymer and 7% trade mark that viscosity by 90% is 10,000mPa.s are A-200 is in room
Temperature is lower to be uniformly mixed, and 3%NaOH is added, and 6h is then kept at 280 DEG C, negative pressure state is remained in system, with removing
Low molecule.It is cooled to room temperature, obtains active matter B.
Embodiment 3:
The preparation of active matter
The white carbon black that the dimethyl silicone polymer and 3% trade mark that viscosity by 95% is 500mPa.s are A-200 is in room temperature
It is lower to be uniformly mixed, and 2%NaOH is added, 3h is then kept at 80 DEG C, negative pressure state is remained in system, to remove low point
Son.It is cooled to room temperature, obtains active matter C.
Embodiment 4:
The preparation of active matter
The white carbon black that the dimethyl silicone polymer and 5% trade mark that viscosity by 92% is 8,000mPa.s are A-200 is in room
Temperature is lower to be uniformly mixed, and 3%NaOH is added, and 7h is then kept at 240 DEG C, negative pressure state is remained in system, with removing
Low molecule.It is cooled to room temperature, obtains active matter D.
Embodiment 5:
According to the method for Si―H addition reaction, the silicon polyethers such as flowering structure is prepared:
Silicon polyethers | E | F | J | I |
R3 | —H | —CH3 | —CH3 | —COCH3 |
x | 15 | 160 | 90 | 450 |
y | 4 | 45 | 26 | 38 |
z | 3 | 5 | 4 | 6 |
g | 5 | 32 | 13 | 25 |
h | 2 | 15 | 9 | 17 |
Embodiment 6:
Using fatty alcohol as initiator, the specific structure of the higher aliphatic polyethers of synthesis is as follows:
Embodiment 7:
The preparation of lotion
At room temperature, active material, higher aliphatic polyethers, silicon polyethers are sufficiently mixed 20min under stiring;After the completion will
The temperature of above-mentioned system is increased to 60 DEG C, then, keeps system temperature, is slowly added into water, and improving mixing speed makes it by W/O
Type lotion becomes O/W type emulsion inverse, continues to add water to required mass concentration, is 50%;Thick lotion by colloid mill into
The emulsification of one step;Finally the lotion W that solid content is 28% is diluted to acrylic acid viscous water.
Embodiment 8:
The preparation of lotion
At room temperature, active material, higher aliphatic polyethers, silicon polyethers are sufficiently mixed 25min under stiring;After the completion will
The temperature of above-mentioned system is increased to 80 DEG C, then, keeps system temperature, is slowly added into water, and improving mixing speed makes it by W/O
Type lotion becomes O/W type emulsion inverse, continues to add water to required mass concentration, is 60%;Thick lotion by colloid mill into
The emulsification of one step;Finally the lotion Q that solid content is 35% is diluted to acrylic acid viscous water.
Embodiment 9:
The preparation of lotion
At room temperature, active material, higher aliphatic polyethers, silicon polyethers are sufficiently mixed 30min under stiring;After the completion will
The temperature of above-mentioned system is increased to 70 DEG C, then, keeps system temperature, is slowly added into water, and improving mixing speed makes it by W/O
Type lotion becomes O/W type emulsion inverse, continues to add water to required mass concentration, is 50%;Thick lotion by colloid mill into
The emulsification of one step;Finally the lotion K that solid content is 30% is diluted to acrylic acid viscous water.
Comparative example 1:
The preparation of lotion
At room temperature, active material, emulsifier, silicon polyethers are sufficiently mixed 35min under stiring;After the completion by above-mentioned system
Temperature be increased to 65 DEG C, then, keep system temperature, be slowly added into water, improving mixing speed becomes it by w/o type lotion
For O/W type emulsion inverse, continue to add water to required mass concentration, is 50%;Thick lotion is further emulsified by colloid mill;
Finally the lotion R that solid content is 28% is diluted to acrylic acid viscous water.
Comparative example 2:
The preparation of lotion
At room temperature, active material, emulsifier, silicon polyethers are sufficiently mixed 40min under stiring;After the completion by above-mentioned system
Temperature be increased to 75 DEG C, then, keep system temperature, be slowly added into water, improving mixing speed becomes it by w/o type lotion
For O/W type emulsion inverse, continue to add water to required mass concentration, is 60%;Thick lotion is further emulsified by colloid mill;
Finally the lotion S that solid content is 35% is diluted to acrylic acid viscous water.
Comparative example 3:
The preparation of lotion
At room temperature, active material, higher aliphatic polyethers, silicon polyethers are sufficiently mixed 25min under stiring;After the completion will
The temperature of above-mentioned system is increased to 70 DEG C, then, keeps system temperature, is slowly added into water, and improving mixing speed makes it by W/O
Type lotion becomes O/W type emulsion inverse, continues to add water to required mass concentration, is 50%;Thick lotion by colloid mill into
The emulsification of one step;Finally the lotion O that solid content is 30% is diluted to acrylic acid viscous water.
Specific gravity relationship between 1 active matter of table and solid content
W | Q | R | S | K | O | |
Active matter proportion | 67.9% | 71.4% | 67.9% | 51.4% | 70% | 50% |
The performance test of 2 lotion of table compares
From the point of view of comprehensive Tables 1 and 2, the stabilization of organic silicon emulsion can largely be improved by introducing higher aliphatic polyethers
Property;Higher aliphatic polyethers is added, specific gravity shared by active matter can also be improved, to reduce making for silicon polyethers and emulsifier
With.
Claims (5)
1. it is a kind of improve stability of organic silicone emulsion method, it is characterised in that: include: active material, higher aliphatic polyethers,
Emulsifier and Siloxane-Oxyalkylene Copolymers;
The described method includes:
R1: active material, higher aliphatic polyethers, emulsifier, silicon polyethers are sufficiently mixed 10-50min under stiring, preferably
15min-30min;
R2: completing that the temperature of above-mentioned system is increased to 55 DEG C -85 DEG C after above-mentioned R1, then keep system temperature, slowly plus
Enter water, improving mixing speed makes it become O/W type emulsion inverse from w/o type lotion, continue to add water to required mass concentration,
Generally 40%-70%, preferably 50%-65%;
R3: thick lotion is further emulsified by colloid mill in above-mentioned R2, is finally diluted to required emulsion concentration with viscous water.
2. a kind of method for improving stability of organic silicone emulsion according to claim 1, it is characterised in that: the active material
It include: polysiloxane, hydrophobic particles and catalyst;The general structure of the polysiloxane is as follows: RaSiO (4-
a)/2;
Wherein, R is substituted or non-substituted monovalent hydrocarbon, and carbon atom number 1-20, these groups include alkyl such as methyl, second
Base, propyl, isopropyl, butyl, isobutyl group;Aryl (phenyl, tolyl, benzyl) and alkylene (including vinyl, propylene
Base);
The hydrophobic particles mainly have silicon, magnesium, zinc, the aluminum oxide of surface hydrophobicity of the partial size less than 25 μm;
The catalyst be broken by polysiloxane chain so that between polysiloxanes and silica further occurrence react,
Further increase the hydrophobicity of hydrophobic silica;
The preparation process of the active material is as follows: being first uniformly mixed polysiloxanes and silica at room temperature, to keep filling
Then tap touching is warming up to reaction temperature, reaction temperature is 50-300 DEG C, and catalyst reaction 2-8h is added, end of reaction drop
It warms to room temperature up to active material.
3. a kind of method for improving stability of organic silicone emulsion according to claim 1, it is characterised in that: the higher aliphatic
Alcohol polyethers is occurred in the catalysis of catalyst and ethylene oxide (EO), propylene oxide (PO) poly- using higher aliphatic as initiator
The polymer that reaction obtains is closed, general formula is as follows: R1O (EO) m (PO) nH;
Wherein, R1 is the initiator of higher aliphatic polyethers, and R1 is alkyl, and carbon atom number is the linear chain or branched chain of 12-24
Alkyl, including dodecyl, myristyl, cetyl, octadecyl and docosyl, R1 are that carbon atom number is 16-
20 straight chained alkyl, m, n are the degree of polymerization in formula, the integer that integer that m is 5-50, n are 10-80;
According to the mass fraction, the active material is 100%, and the higher aliphatic polyethers is selected as 5-30%.
4. a kind of method for improving stability of organic silicone emulsion according to claim 1, it is characterised in that: the emulsifier packet
Include nonionic surfactant, anionic surfactant, cationic surfactant and amphoteric surfactant;
The nonionic surfactant used is one or more mixture, usually based on mass parts score, the active matter
Matter is 100%, and emulsifier is selected as 0-30%.
5. a kind of method for improving stability of organic silicone emulsion according to claim 1, it is characterised in that: described polyether-modified
Polysiloxanes is to occur what addition reaction was prepared under the effect of the catalyst by hydrogen containing siloxane and unsaturated polyether;Institute
Stating dynamic viscosity of the silicon polyethers at 25 DEG C is 10-30,000mPa ﹒ s, and the structural formula of silicon polyethers is as follows: MDx (CH3GSiO) yM;
Wherein, it is chain link R22SiO2/2 that alphabetical M, which represents chain link R23SiOl/2, D in organic siliconresin, and the R2 of two structural formulas takes
It is identical to be worth range;G is polyether group, is indicated with general structure the following:
—(CH2)z(EO)g(PO)hR3;
R3 is-H or-CH3 or-COCH3 in formula;Above-mentioned each structural formula subscript x, y, z, g, h are the degree of polymerization, and x is 10-500's
Integer;Y is the integer of 1-50;Z is the integer of 2-6;G is 1-36 integer;H is the integer of 0-20;
According to the mass fraction, the active material is 100%, then silicon polyethers is selected as 5-30%.
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CN113461970A (en) * | 2021-07-26 | 2021-10-01 | 浙江新安化工集团股份有限公司 | Organic silicon wax emulsion and preparation method thereof |
WO2022001575A1 (en) * | 2020-06-30 | 2022-01-06 | 江苏四新科技应用研究所股份有限公司 | Organosilicone emulsion and preparation method |
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WO2022001575A1 (en) * | 2020-06-30 | 2022-01-06 | 江苏四新科技应用研究所股份有限公司 | Organosilicone emulsion and preparation method |
CN113461970A (en) * | 2021-07-26 | 2021-10-01 | 浙江新安化工集团股份有限公司 | Organic silicon wax emulsion and preparation method thereof |
CN113461970B (en) * | 2021-07-26 | 2022-07-12 | 浙江新安化工集团股份有限公司 | Organic silicon wax emulsion and preparation method thereof |
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