A method of producing emulsions with a high content of the internal phase and latexes based on them

 

(57) Abstract:

The invention provides a method of obtaining emulsions with a high content of the internal phase without phase inversion, which involves the following stages: a) the continuous introduction of dispersant in the presence of an emulsifying and stabilizing amount of a surfactant to the liquid flow of the continuous phase, with a data rate R1and liquid flow of the dispersed phase with a flow rate of R2; and b) mixing the combined flows at the speed of mixing, fairly constant for the formation of emulsions with a high content of the internal phase without phase inversion; the ratio R2: R1covers the interval, the lower limit of which is determined by the point at which the volumetric average particle size of the emulsion with a high content of the internal phase corresponds to the beginning of the inversion depending on the ratio R2: R1and the upper boundary of which is set slightly smaller than R2: R1where there is a phase inversion of the emulsion. According to the method of the present invention can be obtained monodisperse latexes with particle size of about microns, which are used especially in the field of coating, where neophobes.p. f-crystals, 4 Il.

The invention relates to a method of producing emulsions with a high content of the internal phase and articial latexes based on them.

In conventional emulsions, the dispersed phase contains a sphere having a volume content of less of 0.74, which corresponds to the volumetric content for the most compact arrangement of spheres with equal radii. However, for emulsions with a high content of the internal phase (SWF) of the dispersed phase may have a volumetric content of above 0,99. The continuous phase in such cases forms a thin liquid film, which shares many-sided cells, and the stabilization of SWF-emulsions provides adsorption on the surface of cells surfactants of the continuous phase. Such VSWP-emulsion, as is known, can be used as precursors of polymers with high molecular weight, composites and membranes for separation systems (see Ruckenstein et al., J. Colloid Interface Science, Vol. 133, N 2, p. 432 (1989)).

A known method of obtaining SWF-emulsions in a continuous way. For example, in U.S. patent 4018426 (Mertz et al.) disclosed is a system for continuously producing emulsions with SWF, in which two precisely measured phase (internal phase and reversible phase, polluciah from 95:5 to 75: 25 wt%. the ratio of internal phase to reversible phase. This system provides the mixing means, which receives separate threads internal phase and reversible phase and which freely distributes the internal phase in the reversible phase in a stepwise progression. This stepwise progression is implemented by placing a plate having multiple holes with gradually increasing size, which serve to speed the distribution of gradually increasing internal phase in the external phase before the final mixture reaches the outlet. The emulsion obtained using the systems offered Mertz and others described as emulsions intended for use in pharmaceutical and food industries and in firefighting. Develop a simple means of obtaining SWF-emulsions can lead to certain success.

In the quotation above link is not indicated for use SWF-emulsions for artificial latexes. Artificial latex is usually prepared through the following stages: 1) preparation of a solution of polymer or copolymer in a volatile organic solvent; 2) emulsifying the solution in water and aqueous emulsifier; 3) removal is necessary. Getting artificial latexes described in U.S. patent 3360599, 3503917, 4123403 and 5037864.

At the stage of emulsification, and adding water when obtaining artificial latex by the method of phase inversion of water and the emulsifying agent is usually added slowly to the polymer solution under high shear force to achieve the correct ratio of water and polymer solution, which is usually in the range from 1:10 to 4:1. Also known continuous methods. For example, in European patent application 0283247 A2 describes a continuous method of dispersing hydrophobic substances in water at elevated temperature and elevated pressure to get artificial latex having a particle size less than 0.5 micron.

There remains a need in obtaining monodisperse latexes having a submicron particle size, especially in the area of the coating where it is necessary to have a controlled particle size, to minimize oiling and to increase the stability of the latex.

The present invention provides a method of obtaining emulsions with a high content of the internal phase without phase inversion, which involves the following stages:

a) continuously merging into a disperser in the presence of emulsifying and stabiliziruyushchego flow of the dispersed phase, with flow rate 2;

b) mixing the merged streams with sufficient shear force and at a fairly constant relation R2:R1for the formation of emulsions with a high content of the internal phase without phase inversion or manual distribution of the internal phase in the external phase;

where the ratio R2:R1is the interval at which the polydispersity of the emulsion with a high content of the internal phase is not more than 3.

Another object of the present invention is a method for emulsion with a high content of the internal phase without phase inversion, which involves the following stages:

a) continuously introducing a dispersant in the presence of an emulsifying and stabilizing amount of a surfactant, the liquid flow of the continuous phase, with a flow rate of R1and liquid flow of the dispersed phase with a flow rate of R2;

b) mixing the combined flows with the intensity of mixing, fairly constant for the formation of emulsions with a high content of the internal phase without phase inversion;

where the ratio R2:R1covers the interval, the lower limit of which is determined by the point where the medium is the value from the ratio R2:R1and the upper limit is set slightly less than the ratio R2: R1where there is a phase inversion emulsion with a high ratio of the dispersed phase, with the additional condition that the average particle size of not higher than 1.9 μm.

The method of the present invention can be obtained monodisperse particles of submicron size.

In Fig. 1 shows the profile of the distribution of particle sizes and polydispersity particles SWF-emulsion obtained by the method of the present invention, as a function of the velocity ratio of the dispersed phase and continuous phase R2:R1where the continuous phase is water, the dispersed phase of ethylene-octenoyl elastomer ENGAGETMX (trademark of the Dow Chemical Company, 24% of the weight. toluene based on the total weight of copolymer and solvent), and the surfactant is a 4% weight. oleate sodium based on the weight of the elastomer.

In Fig. 2 shows a profile similar to those shown in Fig. 1, but where the continuous phase is a water-dispersed phase - tribocorrosion VECTORTM4211D SIS (trade mark firm Dexco Polymer, 35% weight. toluene based on the total weight of polymer and solvent), and the P> 214 (trade mark of the company Hercules, Inc.) based on the total weight of the copolymer.

In Fig. 3 shows a profile similar to those shown in Fig. 1, but where the continuous phase is water, the dispersed phase is polystyrene, STYRONTM680 (trademark of the Dow Chemical Company, 40% weight. toluene based on the total weight of polymer and solvent), emulsified with 4% weight. surfactants RHODAPEXTMCO-436 (trademark of the firm Rhone-Poulence) based on the total weight of the polystyrene.

In Fig. 4 shows a profile similar to those shown in Fig. 1, but where the continuous phase is a water dispersed phase epoxy resin D. E. RTM331 (trade mark of Dow Chemical Company), and the surfactant is a 4% weight. surfactants RHODAPEX CO-436 based on the total weight of the epoxy resin.

SWF-emulsion of the present invention is produced by continuous draining in the dispersing device in the presence of an emulsifying and stabilizing amount of a surfactant (surfactant) liquid flow of the continuous phase, with a data rate R1and liquid flow of the dispersed phase with a rate R2; and mixing merged Potin "liquid flow continuous phase" is used to denote the current of fluid, which becomes the continuous phase. Similarly, the term "liquid flow of the dispersed phase" is used to denote the current of the liquid, which becomes the dispersed phase.

Liquid flows continuous phase and the dispersed phase sufficiently necesiary with each other, so that they can be emulsify. In accordance with one aspect of the method of the present invention the ratio R2:R1is determined by the interval, where the polydispersity of the particles SWF-emulsion does not exceed 3. In the present invention the term "polydispersity" is used to denote the relationship volumetric average diameter and srednecenovogo particle diameter or Dv/Dn. The term "particles" is used to refer to particles or drops.

In the graph of Fig. 1 point A represents the point at which a volumetric average particle size SWF-emulsions corresponds to the beginning of the inversion depending on the ratio R2:R1before reaching the actual minimum, indicated by point B. Point A is a lower bound of the ratio R2:R1. The plot on the chart enclosed between points a and B represents the area where the volumetric average particle size and/or polydispersity of Cam and from this point to the point C, the particle size and the polydispersity is not essentially depend on the ratio R2:R1. When the ratio R2/R1higher the ratio R2:R1at the point C is the phase inversion that is detected by a rapid increase in particle size and polydispersity SWF-emulsions in the field from point C to point D. the Preferred ratio of dispersed phase to continuous phase for the example shown in Fig. 1, is in the range from 10:1, preferably from 15: 1, more preferably from 20:1 to 60:1, more preferably up to 55:1.

For example, in Fig. 2, the preferred ratio of dispersed phase to continuous phase is from 10:1, preferably from 25:1 to 40:1, more preferably up to 35:1.

For example, in Fig. 3, the preferred ratio of dispersed phase to continuous phase is from 15:1, preferably from 25:1 to 50:1.

In the example of Fig. 4 as the dispersed phase used epoxy resin D. E. RTM331 (trade mark of Dow Chemical Company) without solvent for the resin. In this case the preferred ratio of dispersed phase to continuous phase is from 6:1, preferably from 8:1 to 14:1, preferably up to 13:1.

Surprisingly, VSWP-emulsion produced by the method of the present invention without phase treatment or speed distribution of the treatment SWF-emulsions, and it is done without manual distribution, leading to phase inversion.

Preferably the ratio R2:R1is that the polydispersity is not more than 2.0, more preferably not more than 1.5, and even more preferably not more than 1.2, and most preferably not more than 1.1. Permissible deviation of the velocity of each stream depends, in part, on the nature of the dispersed and continuous phases, as well as dispersant used to obtain SWF-emulsions. Preferably this deviation does not exceed 10%, more preferably 5% and most preferably 1%. Preferably the average particle size SWF-emulsion does not exceed 2 μm, more preferably 1.5 μm and most preferably is not more than 1.0 μm.

The preferred ratio R2:R1depends on a number of factors, including the composition of the phases, the type and amount of surfactant used to stabilize SWF-emulsions and the temperature at which the emulsion.

Continuous phase and the dispersed phase are liquids which are sufficiently necesiary with each other to form a stable SWF-emulsion in the presence rises the values of homogeneous solution, which can be delivered by the pump through the pipeline. The fluid may be undiluted (that is liquid at room temperature), melt (that is liquid at temperatures above room temperature), solid or neptunemay pump liquid that is dissolved in the solvent.

Preferably the continuous phase is an aqueous phase and the dispersed phase contains a polymer and optionally a solvent for the polymer. Acceptable solvents include, but are not limited to, toluene, cyclohexane and methylene chloride. An example of a class of polymers that can be used in the method of the present invention is tribocorrosion containing polymer block of alkanolamides hydrocarbon and a polymer block of a conjugated diene. Triblocaltara well known and can be prepared by any acceptable means, which are described in U.S. patents 3135716, 3150209, 3496154, 3498960, 4145298 and 4169115.

Examples alkanolamides hydrocarbons include alkyl substituted styrene, preferably styrene, - methylsterol and vinyltoluene, with the most preferred styrene. Preferred paired danami are C4-C8- conjugate diene,the most preferred 1,3-butadiene and isoprene.

To obtain SWF-emulsions according to the method of the present invention can also be used polyolefins, such as polypropylene, polyethylene and their copolymers and blends, as well as ethylene-propylene-diene terpolymer. Preferred olefin polymers are linear high density polyethylene (HDPE), heterogeneously branched linear low density polyethylene (LLDPE) such as polyethylene resin DOWLEXTM(trade mark of Dow Chemical Company), heterogeneously branched polyethylene of low density (PESIT), such as ATTANETM(trade mark of Dow Chemical Company), homogeneous branched, linear ethylene-olefin copolymers, such as TAFMERTM(trade mark of Mitsui PetroChemicals Company Limited and EXACTTM(trade mark company Exxon Chemical Company), which can be obtained according to the description of U.S. patent 3645922; branched homogeneous, essentially linear ethylene/-olefin polymers such as a polyolefin plastomer brand AFFINITYTMand polyolefin elastomers brands ENGAGETM(trademark of Dow Chemical Company), which can be obtained, for example, by the method described in U.S. patent 5272236 and 5278272; and the ethylene polymers of high density, obtained by free-radical PE as PRIMACORTM(trade mark of Dow Chemical Company), ethylenevinylacetate copolymers (EVA), such as polymers ESCORENETM(trademark company Exxon Chemical Company) and ELVAXTM(trade mark of company E. I. du Pont de Nemours & Co.).

Preferred essentially linear ethylene/-olefin polymers have a density (measured in accordance with ASTM D-792) of not less than 0,850, more preferably not less than 0,855 and more preferably not less than 0,860 g/cm3but not more than 0,965, more preferably not more than 0,880 and most preferably not more than 0,875 g/cm3the ratio of mass-average molecular weight to srednecenovom molecular weight (Mw/Mn) from 1.5 to 3.0; a melt index (measured in accordance with ASTM D-1238 (190/2.16) not less than 0.1, more preferably not less than 0.5 and most preferably not less than 1 g/10 minutes to not more than 500, more preferably not more than 100, even more preferably not more than 70, and most preferably not more than 10 g/10 min; and the ratio of I10/I2from 6 to 20, more preferably up to 14 (measured in accordance with ASTM D-1238 (190/10)).

Other examples of polymers that may be used in the present is here, epoxy resins, polystyrenes, polyetherimide, polycarbonates and polyurethanes.

Naphthenic and paraffinic hydrocarbons can also be used in the present invention.

Emulsion SWF can be obtained by the method of the present invention even in the absence of polymers. For example, solvents, poorly miscible with water, such as toluene, methylene chloride, cyclohexane, and petroleum ethers can form VSWP-emulsion with water. Additionally, there may be used monomers, such as styrene or acrylate monomers.

Continuous and dispersed phase are equivalent. For example, water flow and the flow of oil that is poured and mixed in the presence of acceptable surfactant at a ratio of flow rates water:oil 20:1, can form a system with a continuous oil phase. On the other hand, water flow and oil flow, which is poured and mixed in the presence of the same or different surfactants, preferably in the presence of another surfactant, at a ratio of flow rates of 1:20, can provide the system with continuous water phase. Although the continuous phase or the dispersed phase is preferably water, more preferably water is the continuous phase, Reborrowed with a pump. The viscosity of the phases can be controlled, for example, by adding a solvent or temperature change. Thus, the solid substance or another polymer of the dispersed phase, which cannot be pumped, it is possible to give this ability due to the dissolution of the polymer in sufficient amount of solvent for the polymer. You can also get the opportunity to use the pump for feeding solids or neptunemay pump fluid through the temperature control.

Surface-active substance (SAS) used to obtain emulsions with SWF, may be anionic, cationic or non-ionic, or their combinations. Usually the higher the surfactant concentration leads to a smaller particle diameter, but at too high concentrations of surfactants has a negative effect on product properties, such as, for example, a film obtained from the emulsion. The concentration of surfactant should be sufficient for the formation of the emulsion and its subsequent stabilization and preferably is in the range of from 0.1, more preferably between 0.5 and most preferably from 2 to 15, more preferably up to 6 and most preferably up to 4 wt%. based on the weight of the dispersed phase. Surfactants can be added to the initial Stausee device as a third stream. Preferably the surfactant is added to the dispersed phase before mixing of the two phases.

Example of an acceptable class of surfactants are sulfates of ethoxylated phenol having the formula X-pH-O-(CH2-CH2-O)n-SO3-,Z-where X represents a linear or branched C6-C18is an alkyl group, preferably octyl, nonyl or lauryl, more preferably octyl or nonyl, most preferably nonyl; f represents a phenylene, preferably p-phenylene; n takes values from 4 to 32, preferably from 4 to 12; Z is a sodium, potassium or ammonium, preferably ammonium. The majority of the preferred and more preferred sulfates ethoxylated phenol is commercially available products, for example, ammonium salt poly(oxy-1,2-atandi-yl) - sulfo-(Nonylphenol).

Other acceptable classes of surfactants include, but are not limited to, salts of fatty acids and alkali metals, such as oleates and stearates of alkali metals; polyoxyethylene nonionic compounds; laurilsulfate alkali metals; Quaternary ammonium surfactant; alkylbenzenesulfonate alkali metals, such as dodecylbenzenesulfonate sodium and m is to be used to produce emulsions with SWF are but not limited to, a rotating shaft disperser bag of the type described in U.S. patent 4123403 (Warner and others ); the stator-rotor mixer with a high shear force; extruder or centrifugal pump head.

The latexes prepared from SWF-emulsions

The latex obtained from SWF-emulsions by combining the emulsion with an acceptable amount of liquid, which is the continuous phase, or liquid that is compatible with the continuous phase and which does not violate the integrity of the particles. When the continuous phase is water, the latex is usually prepared by adding water to SWF-emulsion. It is more preferable to get latex on the continuous scheme by passing the emulsion SWF and water through any acceptable item for dilution, for example, through the centrifugal pump head.

If the dispersed phase of the emulsion with SWF obtained by dissolving a solid substance or a viscous fluid in a suitable solvent, usually after cooking latex solvent, it is desirable to remove. However, if the dispersed phase does not contain solvent, latex can be prepared by simple dilution SWF-emulsions. In this event, the latex is more cost effective that are missing.

You can also obtain a latex having a wide distribution of particle sizes, by combining the emulsion with SWF (or derived from these latexes) with different average particle size. Latexes having a wide distribution of particle sizes, can be particularly useful when it is desirable increase in the content of solid components in the latex while maintaining a low viscosity.

You can also prepare the latexes with many dispersed phases.

It is established that finds application film may be made of latex, obtained on the basis of SWF-emulsions of the present invention. For example, a substantially linear olefin polymer described herein, as it forms a film of almost the same thickness throughout the basis. This film has useful physical properties such as high tensile strength, and can be obtained at any temperature suitable for obtaining the integral of the film, usually in the range of from 25, more preferably from 50 to 150oC, more preferably to 100oC.

The latex based emulsion with SWF obtained by the method of the present invention can be used in cases where commonly used metals, fabric or paper; or the latex may be applied to the form for the manufacture of gloves or condoms. Latex can also be used for adhesives, paints, sealants, putties or bases carpet.

The following example explains the invention and does not limit its scope.

EXAMPLE

A method of obtaining a dispersion with continuous water phase

Ethylene-octenoyl elastomer, the characteristic of which is shown in Fig. 1, is dissolved in toluene to obtain 24% (wt.) the solution is based on the total weight of polymer and solvent. To the resulting solution add sodium oleate (4% weight. based on the weight of the elastomer). This solution is the dispersed phase. The dispersed phase is continuously served by the pump through the sleeve of stainless steel tube with an inner diameter of 1.27 cm, attached to T-shaped profile, at the constant speed of 30 g/min. at the same time the pump serves water (continuous phase) through the sleeve of stainless steel tube with an inner diameter of 0,318 cm, attached to T-shaped profile, at constant speed, which can vary from 6.0 to 0.35 g/ min Two streams merge and blend with each other through the use of nanodesu tube 1.27 cm stainless steel and operates at 7400 rpm Get the emulsion SWF, in which the ratio of dispersed phase to continuous phase is in the range from 10:1 to 60:1 (i.e. the velocity of flow is constant in the interval from 0.5 to 3 g/min). Emulsion with SWF diluted with water and determine the particle size and polydispersity using a light-scattering particle size analyzer Coulter LS 130. From the prepared latex on a rotary evaporator to remove the toluene and again measure the particle size and polydispersity. Get the same result. The solids content was adjusted to 55% due to the removal under vacuum of the water.

1. The way to obtain emulsions with a high content of the internal phase, which involves the following stages: a) the continuous introduction of dispersant in the presence of an emulsifying and stabilizing amount of a surfactant, the liquid flow of the continuous phase, with a flow rate of R1and liquid flow of the dispersed phase with a flow rate of R2b) mixing the combined flows at the speed of mixing, fairly constant for the formation of emulsions with a high content of the internal phase without phase inversion, where the ratio R2: R1covers the interval, the lower limit of which is determined by the point at which depending on R2: R1and the upper boundary of which is set slightly less than the ratio R2: R1where is phase inversion of the emulsion.

2. The method according to p. 1, characterized in that the ratio R2: R1is the interval at which the polydispersity of the particles of the emulsion with a high content of the internal phase is less than 3.

3. The method according to p. 1 or 2, characterized in that the ratio R2: R1is the interval at which the polydispersity of the particles of the emulsion with a high content of the internal phase is less than 2, and the volumetric average particle size is not more than 1.9 μm.

4. The method according to any of paragraphs.1 to 3, characterized in that the ratio R2: R1is the interval at which the volumetric average particle size is not more than 1 μm.

5. The method according to any of paragraphs.1 to 4, characterized in that the continuous phase is an aqueous phase.

6. The method according to any of paragraphs.1 to 4, characterized in that the continuous phase is non-aqueous phase.

7. The method according to any of paragraphs.1 - 6, characterized in that the dispersed phase contains a copolymer of a polymer block of alkanolamides hydrocarbon and a polymer block of suprarenal; or polyurethane.

8. The method according to p. 7, characterized in that the polyolefin contains a homogeneous, statistical, semi-crystalline ethylene--olefin copolymer with a narrow distribution of molecular weight or a substantially linear ethylene/-olefin copolymer having a density of from about 0,850 to 0,965 g/cm3the relation Mw/Mnapproximately 1.5 to 3.0, a melt index from about 0.1 to 100 g/10 min and the ratio of I10/I2from about 6 to 20.

9. The method according to p. 8, wherein the ethylene/-olefin copolymer is an ethylene/1-octenoyl copolymer, having a density of from about 0,855 to 0,875 g/cm3and a melt index from 0.5 to 70 g/10 min.

10. The method according to any of the p. 8 or 9, characterized in that the ratio R2: R1is in the range from 10 : 1 to 60 : 1.

11. The method according to any of paragraphs.8 to 10, characterized in that the ratio R2: R1is in the range from 20 : 1 to 55 : 1.

12. The method according to p. 7, characterized in that the dispersed phase contains a copolymer of a polymer block alkanolamides hydrocarbon.

13. The method according to p. 12, characterized in that the copolymer of the polymer block alkanolamides in the range from 10 : 1 to 40 : 1.

14. The method according to any of the p. 12 or 13, characterized in that the ratio R2: R1is in the range from 25 : 1 to 35 : 1.

15. The method according to p. 7, characterized in that the dispersed phase contains epoxy resin, and the ratio R2: R1is in the range from 6 : 1 to 14 : 1.

16. The method according to p. 7, characterized in that the dispersed phase contains polystyrene, and the ratio R2: R1is in the range from 15 : 1 to 50 : 1.

17. The method according to any of paragraphs.1 to 16, characterized in that the surfactant comprises a combination of surfactants selected from anionic, cationic and nonionic surfactants.

18. The method according to any of paragraphs.1 to 16, characterized in that the surfactant is a salt of a fatty acid and an alkali metal, polyoxyethylene non-ionic compound, lauryl alkali metal, Quaternary ammonium surfactant, Las alkali metal or alkaline soap modified resin, or a combination thereof.

19. The method according to any of paragraphs.1 - 5 and 7 - 18, which, after stage (b) additionally includes the stage of dilution of the emulsion with a high content inside is the obtaining of floor coverings, coatings for wood, automotive coatings, coatings for steel, coatings for paper, gloves, bases carpets, adhesives, sealants, putty, or a condom, obtained by the method described in paragraph 1.

 

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