CN101298027A - Method for dispersing highly viscous organosilicon mixture - Google Patents
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- CN101298027A CN101298027A CNA2008100192951A CN200810019295A CN101298027A CN 101298027 A CN101298027 A CN 101298027A CN A2008100192951 A CNA2008100192951 A CN A2008100192951A CN 200810019295 A CN200810019295 A CN 200810019295A CN 101298027 A CN101298027 A CN 101298027A
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Abstract
The invention provides a method for dispersing high viscosity of silicone mixtures, which is characterized in that: an emulsion prepared by the method is composed of 5 to 25 percent of high viscosity of silicone mixtures, 4 to 25 percent of a high viscosity of silicone emulsifier, 0 to 15 percent of a normal emulsifier, 1 to 5 percent of a thickener and 60 to 90 percent of water; the preparation method comprises the steps that: (1) the high viscosity of silicone emulsifier, the normal emulsifier and the high viscosity of silicone mixtures are mixed, stirred and heated to the temperature of 50 to 80 DEG C and the heat is preserved for 20 to 60 minutes to guarantee full and even mixing of the silicone mixtures and the emulsifiers; (2) water is added slowly and the mixture is stirred quickly during phase transition to ensure that a W/O type emulsion is changed into an O/W type emulsion, and then water is continued to be added until the quality concentration of a crude emulsion gets to 40 to 60 percent; (3) the crude emulsion is carried out colloid mill to be further emulsified; (4) the mixture is diluted by a thickener aqueous solution. The method can obtain a stable emulsion of high viscosity of silicone mixtures and the storage and application stability of the emulsion are improved.
Description
Technical field
The present invention relates to a kind of method that improves stability of emulsion, the present invention relates to a kind of method that improves the highly viscous organosilicon mixture stability of emulsion more precisely, mainly realize with viscosity higher organosilyl surfactant emulsification highly viscous organosilicon mixture.The present invention relates to the preparation of fine chemicals additive, therefore be under the jurisdiction of technical field of fine chemical preparations.
Technical background
The high-viscosity organosilicon emulsion has very wide range of application, can be used for spinning post-finishing agent, fabric softener, anti-sweat agent, defoamer or the like, and full-bodied dimethicone still is the important component in the shampoo.The dispersion emulsion of highly viscous organosilicon mixture is nothing more than following two kinds of methods preparation, and first kind is that method by polymerization forms, as hydroxy-silicone-oil emulsion; Second kind is the method preparation by machinery, and the used various components such as oil phase component, emulsifying agent and water of preparation emulsion are disperseed by adding modes such as thermal agitation, mechanical shearing, colloid mill, homogenizer.
As function additive, as anti-sweat agent, hydroxy-silicone-oil emulsion or the like, have and much all use highly viscous organosilicon mixture, it is dispersed in the water, form O/W type emulsion.Emulsion stable extremely important, otherwise oil phase component is easy to isolate out from emulsion in the process of transportation or storage, be called phenomenons such as floating oil, layering or breakdown of emulsion this moment, if emulsion is not really stable, under vibration or effect, can occur breakdown of emulsion or floating oil phenomenon very soon, so just be unfavorable for the embodiment of the function of emulsion own, can have influence on other auxiliary agents or final products when serious at salt, therefore, the stability of emulsion is the important evaluation index of emulsion self.At the raising of stability of emulsion, U.S. Pat 4853474 improves the resistance to low temperature of emulsion by crosslinked silicon polyethers, but this method is difficult to control the crosslinking degree of silicon polyethers self, so the stability of emulsion is difficult to guarantee uniformity; The application of the alkyl silicon polyethers that US5451692 introduces in the water-in-oil emulsion preparation, by the introducing of alkyl, improved and oil phase component between compatibility.For defoamer, silicone defoaming agent is the high effective antifoaming agent of present aqueous phase system of generally acknowledging, the scope of application relates to fields such as textile printing and dyeing, paper pulp papermaking, sewage disposal, oil exploitation.The silicone defoaming agent emulsion that US5261927 introduces, the stability of emulsion is assessed by the following method, defoamer is to the detection method of the stability of salt: with the defoamer dilution that is added to the water, defoamer after the dilution is joined in the aqueous sodium persulfate solution, and be heated to 90 ℃, relatively have or not full-bodied material floats on liquid level, the appraisal procedure of the stability of emulsion that US6001887 introduces is emulsion to be packed into place the stability of vibration a period of time comparative emulsion on the horizontal oscillator tube in the container then.Patent CN2006100054663.2 also introduces for the high viscosity mixture and is difficult to emulsification treatment.
Because emulsion is the emulsification by emulsifying agent to be distributed to oil phase component in the water and to form.The kind of oil phase component and viscosity are very important for preparation high stability emulsion.Emulsifying agent is adsorbed on the oil-water interfaces in emulsion, if the amount of emulsifying agent is not enough, then the particle in the emulsion is just bigger, even can not emulsification; On the contrary,, in the process of preparation emulsion, can obtain the emulsion of target grain size, just form desired emulsion if the amount of emulsifying agent is enough.But external environment (temperature, transportation) also is very important to the destruction of stability of emulsion, usually can floating oil, breakdown of emulsion, and be a spontaneous process from this process of thermodynamics.The basic reason that this phenomenon occurs is that emulsifying agent has left oil-water interfaces under the variation of external environment, and the emulsifier concentration of so original tiny oil droplets surface unit area reduces, and oil droplet can spontaneously be gathered into bigger particle.This situation shows particularly outstandingly for the high-viscosity organosilicon oil phase component.
The inventor thinks, from the angle of microcosmic, if emulsifying agent can not leave the surface of oil droplet under extraneous environmental change, the stability of emulsion just can not be affected yet.The present invention is by come dispersing highly viscous organosilicon mixture to solve highly viscous organosilicon mixture stability of emulsion problem with the high-viscosity organosilicon emulsifying agent.
Summary of the invention
The purpose of this invention is to provide a kind of method that improves the high-viscosity organosilicon stability of emulsion, it provides a kind of method of dispersing highly viscous organosilicon mixture more precisely, to reach storage and the stability in use that improves the high-viscosity organosilicon emulsion.
Technical scheme:
A kind of method of dispersing highly viscous organosilicon mixture, it provides a kind of method for preparing stable emulsion with high-viscosity organosilicon composition.Described highly viscous organosilicon mixture, its viscosity are 10,000～1,000,000mPas.Prepared emulsion is made up of highly viscous organosilicon mixture, full-bodied organosilyl surfactant, common emulsifying agent, thickener, water.The method of this dispersing highly viscous organosilicon mixture is characterized in that using full-bodied organosilyl surfactant in the emulsion components, says so more specifically and comes the emulsification highly viscous organosilicon mixture with full-bodied organosilyl surfactant.
Described full-bodied organosilyl surfactant is an organic silicon modified by polyether, is called for short " silicon polyethers ", and its general structure is as follows:
Wherein:
Subscript a, b are 0 or 1 or 2, but a+b is 2; M and n are the degree of polymerization of two silicon chain links in the used full-bodied silicon oil of low hydrogen content of the full-bodied organosilyl surfactant of preparation, and m is 100～2000 integer, and n is 200～1000 integer.The value of m and n should guarantee that the viscosity of the used full-bodied silicon oil of low hydrogen content of the full-bodied organosilyl surfactant of described preparation is 500～15000mPas, and preferred 1000～6000mPas, hydrogen content are 0.01～1.5%, preferred 0.10～1.00%.
R
1For carbon number is 1～18 alkyl, comprise methyl, ethyl, propyl group, isopropyl, butyl, octyl group, iso-octyl, 12 carbon alkyl, tetradecane base, hexadecane base, octadecyl or the like, preferred R
1Be methyl.
R
2For-(O) p (CH
2) the qO-linking group.When p=0, formation be stable Si-C chemical bond, this moment, q was 3～6 integer, preferred q is 3; What form when p=1 is the Si-O-C chemical bond, and this moment, q was 1～8 integer, and preferred q is 3～6.
X, y are the degree of polymerization of oxirane (EO), expoxy propane (PO), and x, y are 0～20 integer, but x, y can not be 0 simultaneously.
R
3Being the polyethers end-capping group, is 1～4 alkyl or short chain organosilicon end capping group for H atom or carbon number.The structural formula of wherein said short chain organosilicon end capping group is as follows:
Wherein, c and d are respectively the degree of polymerization of two chain links, c=0～10, d=1～5, R
4Be H or carbon number 1～20 alkyl, alkyl comprises methyl, ethyl, propyl group, isopropyl, butyl, octyl group, iso-octyl, 12 carbon alkyl, tetradecane base, hexadecane base, octadecyl or the like, preferable methyl.
Described full-bodied organosilyl surfactant is to be made by hydrosilylation or the condensation reaction of silicon hydrogen by full-bodied silicon oil of low hydrogen content and polyethers, and products therefrom also claims " silicon polyethers ", and its viscosity is 5,000～150,000mPas.Prepare the used full-bodied silicon oil of low hydrogen content of full-bodied organosilyl surfactant and adopt high containing hydrogen silicone oil, octamethylcy-clotetrasiloxane (D
4) and HMDO (MM) or 1,3-dihydro tetramethyl disiloxane carries out polymerisation and makes under the effect of acidic catalyst, described acidic catalyst is selected from sulfuric acid, phosphoric acid, solid acid or Emathlite, finish the back catalyst neutralisation at chemical reaction, and then filtration gets final product.
Preparing hydrosilylation or the condensation reaction of silicon hydrogen that full-bodied organosilyl surfactant adopts is to carry out under the condition that catalyst exists, and the hydrosilylation that forms the Si-C key adopts chloroplatinic acid catalyst; The metallic tin catalyst is adopted in the condensation reaction that forms the Si-O-C key, as stannous octoate, dibutyl tin dilaurate etc.Be reflected at and carry out in the solvent or in solvent, do not carry out, if in solvent, generally select atent solvent for use, as benzene,toluene,xylene or the like.Reaction temperature generally is controlled at 70～130 ℃, and the reaction time is 0.5～6h.
Described polyethers is to be initiator with the fatty alcohol, and the mixture with oxirane (EO) and expoxy propane (PO) in reaction under high pressure adds on the fatty alcohol continuously with certain reaction speed, and reaction temperature is generally between 120～150 ℃.If with α-unsaturated fatty alcohol is initiator, just obtain the unsaturated fatty alcohol polyethers, it and full-bodied silicon oil of low hydrogen content generation hydrosilylation obtain the silicon polyethers of Si-C key.If with the saturated fatty alcohol is initiator, promptly obtain the saturated fatty alcohol polyethers, the reaction of it and full-bodied silicon oil of low hydrogen content belongs to condensation reaction, intermolecularly sloughs a hydrogen molecule, forms the silicon polyethers of Si-O-C key.
A kind of method of dispersing highly viscous organosilicon mixture, prepared emulsion, by percentage to the quality, its each component ratio is as follows:
Table 1 emulsion preparation prescription
| Raw material | Ratio | Preferably |
| Highly viscous organosilicon mixture | 5～25％ | 10～20％ |
| The high-viscosity organosilicon emulsifying agent | 4～25％ | 8～17％ |
| Common emulsifying agent | 0～15％ | 0～10％ |
| Thickener | 1～5％ | 2～3％ |
| Water | 60～90％ | 65～80％ |
The method of emulsion preparation mainly comprises " agent-in-oil method " and " agent-in-water method ".The present invention adopts former approach, concrete grammar is as follows: will go up the described high-viscosity organosilicon emulsifying agent of table, common emulsifying agent and highly viscous organosilicon mixture earlier and mix the stirring intensification, temperature is elevated to 50～80 ℃, preferred 60～70 ℃, and be incubated 20～60min, preferred 35～45min makes organosilicon mixture and emulsifying agent fully mix; To wherein slowly adding entry, make the w/o type emulsion fully be transformed into O/W type emulsion then, when phase inversion, stir fast; Continuing to add water then, is 40～60% up to thick quality of the emulsion concentration; By colloid mill, further emulsification reaches required particle diameter up to particle size of emulsion with above-mentioned thick emulsion; Be diluted to certain concentration with aqueous thickener solution again.
The emulsifying agent that above-mentioned preparation method uses comprises high-viscosity organosilicon emulsifying agent and common emulsifying agent, and wherein common emulsifying agent refers to anion emulsifier or nonionic emulsifier, preferred nonionic emulsifier.Be suitable for nonionic emulsifier of the present invention and comprise AEO, aliphatic acid polyethenoxy ether, aliphatic amine polyoxyethylene ether, APES, comprise tween series, this Pan's series, TX series, NPE series, MOA series, OPE series, EL series, stearic acid polyoxyethylene ether ester series particularly.
Method at a kind of dispersing highly viscous organosilicon mixture prepares the thickener that uses in the emulsion, is selected from cellulose ethers, polyvinyl alcohol, mosanom, polyacrylate, polyacrylamide, xanthan gum or card ripple.
If the emulsion of preparation needs long term storage, in the preparation emulsion, add a small amount of bactericide and anticorrisive agent, as clorox, potassium sorbate, s-triazine, triumphant pine etc., addition is 0.05～0.5% of an emulsion gross mass, preferred 0.1～0.3%.
The performance of the organic silicon emulsion of the inventive method preparation is mainly assessed from the following aspects:
(1) water dilution stability:
Join according to 1 part organic silicon emulsion in 99 parts the water, after being uniformly dispersed, observe the liquid level situation.
(2) particle diameter of water diluent:
Join according to 1 part organic silicon emulsion in 99 parts the water, under current intelligence, measure particle size then with laser particle diameter instrument.Then this dilution was placed three days, measured the particle diameter of dilution once more, with incipient result's contrast.
(3) stability of emulsion self:
The stability of emulsion self mainly is that emulsion stoste is stored three days at high temperature (40 ℃), low temperature (3～5 ℃), then according to the method for (1), compares the liquid level situation of dilution.
(4) anti-shear performance of emulsion:
Under the normal temperature, emulsion stoste is placed on the horizontal oscillator tube amplitude with 6cm, the hunting of frequency 30min of 100 times/min, according to the method for (1), the liquid level situation of dilution relatively.
Embodiment
Embodiment 1: serial polyethers synthetic
The polyethers that table 2 is synthetic
| Sequence number | The structural formula of polyethers |
| Unsaturated polyether A | CH 2＝CHCH 2O(PO) 7CH 3 |
| Unsaturated polyether B | CH 2＝CHCH 2O(EO) 7(PO) 5H |
| Unsaturated polyether C | CH 2＝CHCH 2O(EO) 10CH 3 |
| Saturated polyethers D | CH 3CH 2CH 2CH 2O(EO) 10(PO) 5H |
Synthetic method: in the polyether reactant still, add propenyl or butanols and 0.3%KOH catalyst.Continue then to be warming up near 130 ℃,, and then add expoxy propane PO, add back insulation 60min,, obtain colourless viscous liquid with Emathlite decolouring, neutralization and adsorption refining earlier to wherein adding oxirane EO.
Embodiment 2: synthetic full-bodied silicon oil of low hydrogen content
Table 3 synthesizes full-bodied silicon oil of low hydrogen content
Full-bodied silicon oil of low hydrogen content carries out chemical reaction in the above-mentioned raw materials ratio and makes under the effect of acidic catalyst, catalyst is a sulfuric acid, reaction back catalyst neutralisation refilters and gets final product, the high viscosity silicon oil of low hydrogen content S1, S2, S3, the S4 that make respectively in the ratio of table 3.
Embodiment 3: full-bodied organosilyl surfactant (that is: silicon polyethers) synthetic
Can make following silicon polyethers emulsifying agent according to silicon hydrogen addition method or dehydrogenative condensation reaction:
Table 4 synthesizes the silicon polyethers
| S1 | S2 | S3 | S4 | |
| Unsaturated polyether A | S1-A | S2-A | S3-A | S4-A |
| Unsaturated polyether B | S1-B | S2-B | S3-B | S4-B |
| Unsaturated polyether C | S1-C | S2-C | S3-C | S4-C |
| Saturated polyethers D | S1-D | S2-D | S3-D | S4-D |
Embodiment 4: the highly viscous organosilicon mixture preparation
Be prepared as follows organosilicon mixture with reference to the example among the US4639489 1: with 378g viscosity is 100, the dimethicone of 000mPas and 180g viscosity are 10, the end hydroxyl silicone oil of 000mPas and 18g ethyl orthosilicate are put in the reactor bottle, be heated to 130～140 ℃, (Preparation of catalysts: 90g viscosity is 1, and the dimethicone of 000mPas and 10gKOH are at 120 ℃ of reaction 15min to wherein adding the 3g catalyst then.), stir and continue and heat.Be 200m to wherein adding the 30g specific area then
2The white carbon of/g homogenizer homogeneous phaseization.Reactant mixture is heated to 180 ℃, and keeps 4h, and it is organosilicon mixture that cool to room temperature just obtains thick liquid.
Embodiment 5: highly viscous organosilicon mixture prepares the preparation of emulsion E-1
Get the mixture in 100 parts the example 4, then to wherein adding 40 parts of emulsifying agent S1-A, 20 parts of emulsifying agent S1-B and 17 parts of emulsifying agent S1-C and 3 parts of these Pan 85, be warming up to 60 ℃, the frequency stirring 40min with 50Hz makes organosilicon mixture and emulsifying agent fully mix.To wherein slowly adding 100 parts of water, stir fast when phase inversion then, the raising rotating speed is 65Hz, make O/W type emulsion fully be transformed into O/W type emulsion, continue to add 90 parts of water then, this moment, emulsion concentration was 50%, by homogenizer, further emulsification, up to the grain of emulsion through reaching 10～30 μ m.Fast cooling is to normal temperature then, and to be diluted to concentration with 360 parts of acrylic acid viscous waters be 25% emulsion, adds 0.2% clorox and cooks anticorrisive agent.
Embodiment 6: highly viscous organosilicon mixture prepares the preparation of emulsion E-2
Get the mixture in 100 parts the example 4, then to wherein adding 40 parts of emulsifying agent S2-B, 20 parts of emulsifying agent S2-C and 17 parts of emulsifying agent S2-D and 3 parts of these Pan 85, be warming up to 60 ℃, the frequency stirring 40min with 50Hz makes organosilicon mixture and emulsifying agent fully mix.To wherein slowly adding 100 parts of water, stir fast when phase inversion then, the raising rotating speed is 65Hz, make O/W type emulsion fully be transformed into O/W type emulsion, continue to add 90 parts of water then, this moment, emulsion concentration was 50%, by homogenizer, further emulsification, up to the grain of emulsion through reaching 10～30 μ m.Fast cooling is to normal temperature then, and to be diluted to concentration with 360 parts of acrylic acid viscous waters be 25% emulsion, adds 0.2% clorox and cooks anticorrisive agent.
Embodiment 7: the preparation of highly viscous organosilicon mixture emulsion E-3
Get the mixture in 100 parts the example 4, to wherein adding 40 parts of emulsifying agent S3-A, 30 parts of emulsifying agent S3-C and 30 parts of emulsifying agent S3-D, be warming up to 60 ℃ then, stir 40min, make organosilicon mixture and emulsifying agent fully mix with the frequency of 50Hz.To wherein slowly adding 150 parts of water, stir fast when phase inversion then, the raising rotating speed is 65Hz, make O/W type emulsion fully be transformed into O/W type emulsion, continue to add 150 parts of water then, this moment, emulsion concentration was 40%, by homogenizer, further emulsification, up to the grain of emulsion through reaching 5～30 μ m.Fast cooling is to normal temperature then, and to be diluted to concentration with 400 parts of acrylic acid viscous waters be 22% emulsion, adds 0.2% potassium sorbate and cooks anticorrisive agent.
Embodiment 8: the preparation of highly viscous organosilicon mixture emulsion E-4
Get the mixture in 100 parts the example 4, then to this Pan 60 who wherein adds 60 parts of emulsifying agent S4-A, 30 parts of emulsifying agent S4-B, 50 parts of emulsifying agent S4-C and 10 parts, be warming up to 60 ℃, the frequency stirring 40min with 50Hz makes organosilicon mixture and emulsifying agent fully mix.To wherein slowly adding 130 parts of water, stir fast when phase inversion then, the raising rotating speed is 65Hz, make the w/o type emulsion fully be transformed into O/W type emulsion, continue to add 120 parts of water then, this moment, emulsion concentration was 50%, by homogenizer, further emulsification, up to the grain of emulsion through reaching 5～30 μ m.Fast cooling is to normal temperature then, and to be diluted to concentration with 500 parts of acrylic acid viscous waters be 25% emulsion, adds 0.2% potassium sorbate and cooks anticorrisive agent.
Claims (6)
1, a kind of method of dispersing highly viscous organosilicon mixture, it is characterized in that, its preparation emulsion is made up of 5～25% highly viscous organosilicon mixtures, 4～25% full-bodied organosilyl surfactants, 0～15% common emulsifying agent, 1～5 thickener, 60～90% water by mass; Performing step is:
(1) full-bodied organosilyl surfactant, common emulsifying agent and highly viscous organosilicon mixture are mixed stirring and heat up, be warmed up to 50～80 ℃, and be incubated 20～60min, make organosilicon mixture and emulsifying agent fully mix;
(2) then to wherein slowly adding entry, making the w/o type emulsion fully be transformed into O/W type emulsion, stir fast when phase inversion, continue to add water then, is 40～60% up to thick quality of the emulsion concentration;
(3) above-mentioned thick emulsion is passed through colloid mill, further emulsification;
(4) dilute with aqueous thickener solution again.
2, the method for a kind of dispersing highly viscous organosilicon mixture according to claim 1, the viscosity that it is characterized in that described highly viscous organosilicon mixture is 10,000～1,000,000mPas.
3, the method for a kind of dispersing highly viscous organosilicon mixture according to claim 1 is characterized in that described full-bodied organosilyl surfactant is an organic silicon modified by polyether, is called for short " silicon polyethers ", and its general structure is as follows:
Wherein:
Subscript a, b are 0 or 1 or 2, but a+b=2;
Subscript m and n are the degree of polymerization of two silicon chain links, and m is 100～2000 integer, and n is 200～1000 integer;
R
1For carbon number is 1～18 alkyl, preferable methyl;
R
2For-(O) p (CH
2) the qO-linking group, p is 0 or 1, and q is 3～6 integer when p=0, and q is 1～8 integer when p=1;
Subscript x, y are the degree of polymerization of oxirane (EO), expoxy propane (PO), and x, y are 0～20 integer, but x, y can not be 0 simultaneously;
R
3Be the polyethers end-capping group, for H or carbon number are 1～4 alkyl or short chain organosilicon end capping group, the structural formula of wherein said short chain organosilicon end capping group is as follows:
In the said structure formula, c and d are respectively the degree of polymerization of two silicon chain links, c=0～10, d=1～5, R
4For H or carbon number are 1～20 alkyl, preferable methyl;
4, the method for a kind of dispersing highly viscous organosilicon mixture according to claim 3, it is characterized in that described full-bodied organosilyl surfactant is to be made by hydrosilylation or the condensation reaction of silicon hydrogen by full-bodied silicon oil of low hydrogen content and polyethers, its viscosity is 5000～150,000mPas, the viscosity of wherein said full-bodied silicon oil of low hydrogen content is 500～15000mPas, and hydrogen content is 0.01～1.5%.
5, the method for a kind of dispersing highly viscous organosilicon mixture according to claim 1, wherein said common emulsifying agent is anion emulsifier or nonionic emulsifier.
6, the method for a kind of dispersing highly viscous organosilicon mixture according to claim 1, wherein said thickener are selected from cellulose ethers, polyvinyl alcohol, mosanom, polyacrylate, polyacrylamide, xanthan gum or card ripple.
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